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88 RADIOCHEMISTRY, STABLE ISOTOPES, NUCLEAR ANALYTICAL METHODS, GENERAL CHEMISTRY Fig.2. SEM photomicrographs of TiO 2 films on glass derived from (a) ASC-containing sol and (b) conventional sol; (c) spherical powder from ASC-containing sol. because of lower content of nitrates, many of which decomposed during an earlier, low-temperature preparation step: TiO(OH) a -3.5NO 3 -H 2 O + ASC → TiO(OH) a+x -(3.5-y)NO 3 -H 2 O-CO 2 Figure 1 shows XRD patterns of titania gels calcined for 2 h at various temperatures. Formation of crystalline phases of titania and transformation anatase to rutile phases took place at lower temperatures when ASC was added. Temperatures to complete reaction were similar to those <strong>report</strong>ed when organometallic precursors have been used [16-20]. SEM of the TiO 2 films (1-5 µm thick) coated onto glass substrates revealed that the ASC-containing sols produced better morphologies and improved adhesion (Fig.2a,b). There was no significant difference in spherical powders prepared from both types of sol, but it seemed that ASC-based spheres (Fig.2c) were slightly finer and more regular. All products exhibited excellent phase purity. BaTiO 3 For preparation of BaTiO 3 , a key was to maintain sols without precipitation of Ba nitrates. Thermal analysis of two gels prepared with addition of Ba(NO 3 ) 2 and Ba(OH) 2 are shown in Fig.3a. For all gels, the dominant endotherm, observed at ca. 600 o C, could be attributed to melting; smaller endotherms were attributed to decomposition of Ba nitrates. Addition of ASC induced melting at lower temperature. XRD analyses of powders treated to various temperatures indicated that addition of ASC promoted formation of the desired crystalline phase. Nitrates were present from 500 to 570 o C; at 600 o C, all nitrates decomposed over a 2 h period and formation of crystalline BaTiO 3 began. The temperature of formation and crystallization temperatures (Fig.3b) were comparable to what has been <strong>report</strong>ed when organometallic reagents have been used [23]. BiTiO 3 films were prepared on glass and Ag substrates by a dip-coating technique. XRD confirmed good phase purities. SEM revealed various morphologies. The films were generally smooth, but examinations at magnifications of 5000x or above indicated microscopic irregularities. As was found with the TiO 2 films on glass substrates, addition of ACS resulted in minimization of cracks. One presumes lower shrinkage upon firing to be the cause of the improvement. Following our success with production of medium-sized Li 2 TiO 3 spherical particles [1-3], we prepared particles by a similar method from the Fig.3. (a) DTA traces of BaTiO 3 sols with (dashed line) and without (solid line) ASC; (b) XRD patterns after 2 h at various temperatures for ASC-derived BaTiO 3 .
RADIOCHEMISTRY, STABLE ISOTOPES, NUCLEAR ANALYTICAL METHODS, GENERAL CHEMISTRY 89 Fig.4. XRD spectra, intensity (I) in arbitrary units, of (a) SrTiO 3 and (b) CaTiO 3 fired to 800°C, 24 h. Ba-Ti/OH-NO 3 sol. We initially obtained Ba-Ti gel spheres of diameter 1-80 µm, but with Ba loss and a final molar ratio of Ba:Ti=0.2. Per previous successes [1-3], we therefore impregnated the gels with Ba(OH) 2 in a hot solution (90 o C, 25 g Ba/l), followed by vacuum drying, and final thermal treatment. With impregnation, we obtained medium-sized spherical powders (most spheres were 15-30 µm). We have not been able to identify BaTiO 3 spheres of such size in the literature: although fine (diameter
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ANNUAL REPORT 2005 50 years in the
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CONTENTS GENERAL INFORMATION 9 MANA
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DETERMINATION OF CADMIUM, LEAD, COP
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NUCLEONIC CONTROL SYSTEMS AND ACCEL
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GENERAL INFORMATION 9 GENERAL INFOR
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MANAGEMENT OF THE INSTITUTE 11 MANA
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MANAGEMENT OF THE INSTITUTE 13 •
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SCIENTIFIC STAFF 15 5. Danilczuk Ma
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RADIATION CHEMISTRY AND PHYSICS, RA
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20 RADIATION CHEMISTRY AND PHYSICS,
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NUCLEAR TECHNOLOGIES AND METHODS 14
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THE INCT PUBLICATIONS IN 2005 143 T
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THE INCT PUBLICATIONS IN 2005 145 2
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THE INCT PUBLICATIONS IN 2005 163 V
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NUKLEONIKA 169 NUKLEONIKA THE INTER
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NUKLEONIKA 171 7. Influence of time
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INTERVIEWS IN 2005 173 INTERVIEWS I
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CONFERENCES ORGANIZED AND CO-ORGANI
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EDUCATION 209 EDUCATION Ph.D. PROGR
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RESEARCH PROJECTS AND CONTRACTS 211
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RESEARCH PROJECTS AND CONTRACTS IAE
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LIST OF VISITORS TO THE INCT IN 200
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LECTURES AND SEMINARS DELIVERED OUT
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LECTURES AND SEMINARS DELIVERED OUT
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AWARDS IN 2005 221 AWARDS IN 2005 1
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INSTRUMENTAL LABORATORIES AND TECHN
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INDEX OF THE AUTHORS 235 Lisowska H
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