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1.
Aluminium oxides doped with 1% 57Fe were prepared by sol-gel method, and annealed for 3 hours at various temperatures between 550°C and 1100°C. Amorphous phases were obtained below 1000°C, and crystalline α–Al2O3 was formed at 1100°C. Although Al2O3 itself shows diamagnetism, the light doping of Fe ions into aluminium oxide induced a very weak ferromagnetism, but the ferromagnetism disappeared by longer annealing. M?ssbauer spectra were composed of paramagnetic Fe2?+? and Fe3?+? species for samples heated below 750°C, and of paramagnetic Fe3?+? above 850°C, in addition to a magnetic sextet and relaxation peaks of Fe3?+?. The magnetic and quadrupole interactions of the sextet and the relaxation peaks and the density functional calculations suggest that the lightly doped Fe3?+? ions are substituted at Al sites in the Al2O3 lattice.  相似文献   

2.
Magnetic iron nanoparticles immersed in a carbon matrix were produced by a combined process of controlled dispersion of Fe3?+? ions in sucrose, thermal decomposition with simultaneous reduction of iron cores and the formation of the porous carbonaceous matrix. The materials were prepared with iron contents of 1, 4 and 8 in %wt in sucrose and heated at 400, 600 and 800°. The samples were analyzed by XRD, Mössbauer spectroscopy, magnetization measurements, TG, SEM and TEM. The materials prepared at 400° are composed essentially of Fe3O4 particles and carbon, while treatments at higher temperatures, e.g. 600 and 800° produced as main phases Fe0 and Fe3C. The Mössbauer spectra of samples heated at 400° showed two sextets characteristic of a magnetite phase and other contributions compatible with Fe3?+? and Fe2?+? phases in a carbonaceous matrix. Samples treated at temperatures above 600° showed the presence of metallic iron with concentrations between 16?C43%. The samples heated at 800° produced higher amounts of Fe3C (between 20% and 58%). SEM showed for the iron 8% sample treated at 600?C800°C particle sizes smaller than 50 nm. Due to the presence of Fe0 particles in the carbonaceous porous matrix the materials have great potential for application as magnetic adsorbents.  相似文献   

3.
High-temperature in situ Mössbauer spectroscopy measurements (300–950°C) were done on synthetic olivine of composition (Mg0.55Fe0.45)2 SiO4 (=Fa45) in order to study the distribution of Fe2?+? over the M1 and M2 octahedral sites. The spectra are fit with two doublets, which are assigned to Fe2?+? at the M1 (smaller splitting) and M2 sites. The Fe2?+? site-occupancies at M1 and M2, obtained from the Mössbauer relative areas, suggest that Fe2?+? has a slight preference for the M1 site at temperatures below ~500°C, with a tendency of disordering around this temperature. At higher temperatures, Fe2?+? again prefers to occupy the M1 site, where it shows a considerable order at this site up to 750°C. At still higher temperatures, the spectra indicated partial reduction of the Fa-component into metallic iron and the resolution of the doublets was severely deteriorated.  相似文献   

4.
Thermoluminescence (TL), optical absorption (OA), electron spin resonance (ESR) and their relation to point defects in spessartine have been investigated. The TL glow curve presented four peaks at 150, 220, 260 and 335 °C. The 150 and 335 °C TL peaks growth curves presented a linear growth with radiation dose up to about 400 Gy, supralinearity above this dose, and saturation around 800–1000 Gy. The OA spectrum presented allowed spin transition bands due to Fe3+ and Mn2+ in dodecahedral environment. Absorption bands due to ultraviolet charge transfer of Fe3+ in octahedral and tetrahedral positions were also observed. Two ESR, a strong one around g?~?2 due to Fe3+ in octahedral position, and another weaker one at g?~?4 due to Fe3+ in tetrahedral position, have been detected. The effect of high temperature annealing (600–900 °C) before irradiation was also investigated.  相似文献   

5.
States of dilute Fe in SnO2 have been monitored using 57Fe emission Mössbauer spectroscopy following implantation of 57Mn (T 1/2 = 85.4 s) in the temperature range from 143 K to 711 K. A sharp annealing stage is observed at ~330 K where the Fe3?+?/Fe2?+? ratio shows a marked increase. It is suggested that this annealing stage is due to the dissociation of Mn-VO pairs during the lifetime of 57Mn; the activation energy for this dissociation is estimated to be 0.9(1) eV. Fe3?+? is found in a paramagnetic state showing spin-lattice relaxation rates consistent with an expected T 2 dependence derived for a Raman process. In addition, a sharp lined doublet in the Mössbauer spectra is interpreted as due to recoil produced interstitial Fe.  相似文献   

6.
Amorphous layers produced at the surface of iron by B+ and C+ implantation (50 kV, 1×1018 ions cm−2) were analyzed by CEMS. The CEM spectrum of B+ implanted layer was composed of broad doublet and sextet. Spread hyperfine field distribution, P(H), indicates the formation of extremely disordered FeB layer. Annealing at 400°C brought about precipitation of FeB, which was converted to Fe2B by annealing at 500°C. The P(H) for C+ implanted iron was resolved to 3 subpeaks with H values of 11.0, 18.0 and 22.5 T. The amorphous FeC phase was strongly correlated to crystalline Fe5C2 and Fe2C, which precipitated at 300°C and were transformed into Fe3C at 500°C. The amorphous layer disappeared by annealing at 600°C.  相似文献   

7.
Variations in coordination states of extra-framework iron are studied in low iron content ferrisilicates (Si/57Fe ≈ 200) during various in situ treatments. In Fe-LTA complete Fe3+ ? Fe2?+? reversibility is observed. In Fe-MFI extra-framework iron can be stabilized in Fe2?+? state in spite of ambient oxidizing conditions (N2O, 620 K). Further, in Fe-MFI simultaneous stabilization of Fe2?+? and Fe3?+? may take place providing centres for redox catalytic processes.  相似文献   

8.
Sintered plates of alumina have been implanted at room temperature with 110 keV57Fe+ at a dose of 1.2×1017 ions.cm?2. The analysis of the Conversion Electron Mössbauer Spectrum indicated that implantation introduces iron in alumina in three charge state: Fe2+ (two components), Fe4+ and Fe0 (metallic clusters). The evolution of the iron depth distribution during annealings in oxiding or in neutral atmosphere has been followed using the Rutherford backscattering spectroscopy. Up to 800°C the profile as well as the charge states of iron evolve very slowly. A drastic change occurs' for annealing temperature around 1000°C. The total amount of iron is distributed among α-Fe2O3 and α-(Fe1?x Al x )2O3 precipitates. Some scanning electron micrographs have allowed to locate these precipitates. For highest temperature anneals, up to 1600°C, only substitutional iron remain.  相似文献   

9.
Mg oxides doped with 1 % 57Fe were prepared by a sol-gel method, and annealed at various temperatures. Nano-size Mg oxides were characterized by Mössbauer spectrometry, magnetization and XRD measurements. The crystalline size of MgO increases with increase of annealing temperature. Samples annealed at 600 °C and 800 °C gave only doublet peaks of paramagnetic Fe3+ in Mössbauer spectra although Fe3+ doping into MgO induced a distorted structure and showed weak ferromagnetism. It is considered that the magnetic property is due to defect induced magnetism by doping Fe3+ into MgO. For a sample heated at 1000 °C, it is found from low temperature Mössbauer spectra that Fe3+ species are located at the core and shell of fine MgFe2O4 grains and diluted in MgO matrix.  相似文献   

10.
The Fe oxidation degree determined by 57Fe Mössbauer spectroscopy and microprobe was used to characterize fresh and altered phlogopite megacrysts from an evolved carbonatitic kimberlite from northeastern Oman. The Quadrupole splitting (QS) varies between 2.19 and 2.48 mm/s (Fe2?+?) in the fresh phlogopite samples and between 2.40 and 2.47 mm/s in the altered phlogopite samples. The quadrupole splitting of the Fe3?+? doublets varies between 0.66 and 0.85 mm/s in the fresh samples. The altered phlogopite samples show three Fe3?+? doublets; the first show a quadrupole splitting between 0.97 and 1.13, the second quadrupole splitting varies between 0.24 and 0.46 mm/s and the third varies between ??0.23 and ??0.35 mm/s. The phlogopite was observed to have an average Fe3?+?/Fetotal of 35% to 37%, and corresponds to fresh phlogopite. The second one results from the alteration of the first type, and the Fe3?+?/Fetotal ranges between 40% and 57%. Tetrahedral Fe3?+? ions were confirmed in the altered phlogopite samples. Quantitative Fe site distributions can be obtained from room-temperature Mössbauer data if the different recoilless factors for octahedral Fe2?+? and tetrahedral Fe3?+? are considered. The observed isomer shifts are consistent with Mössbauer temperatures of 330 K, reported in the literature for tetrahedral and octahedral Fe3?+? and Fe2?+? in phlogopite. The results are compared to those obtained for natural and synthetic phlogopite from worldwide.  相似文献   

11.
Changes in morphological and magnetic properties of Fe3O4 nanoparticles before and after annealing are investigated in the present work. The nanoparticles are synthesized in a standard capacitively coupled plasma enhanced chemical vapour deposition system with two electrodes using ferrocene as the source compound. Post annealing, due to the sintering process, the particles fuse along with recrystallization. This results in increased size of the nanoparticles and the interparticle interaction, which play a major role in deciding the magnetic properties. X-ray diffraction patterns of the samples before and after annealing indicate a phase change from Fe3O4 to Fe2O3. Annealing at 200 °C causes the apparent saturation magnetization to increase from 6 emu?g?1 to 15 emu?g?1. When annealed at 500 °C, the magnetic properties of the nanoparticles resemble those of the bulk material. The evidence for the transition from a superparamagnetic state to a collective state is also observed when annealed at 500 °C. Variation of the magnetic relaxation data with annealing also reflects the change in the magnetic state brought about by the annealing. The correlation between annealing temperature and the magnetic properties can be used to obtain nanocrystallites of iron oxide with different sizes and magnetic properties.  相似文献   

12.
The kinetics of the nanocrystalline structure formation in the Fe73.5Cu1Nb3Si22.5?xBx (x=6. 7. 8. 9 at. %) was followed during the annealing runs interrupted between 300 and 700°C.57Fe room temperature Mössbauer spectra were taken and complemented by the electrical resistivity and X-Ray diffraction measurements. It has been found that for the 50 K/min temperature increase the formation of the nanocrystalline phase begins above 450°C reaching a maximum around 500°C and is followed by the second stage of crystallization of the disordered intergranular remainder above ca 600°C accompanied by the changes in the occupation of the iron sites in the crystalline α?Fe?Si phase. Thus gained composition-temperature dependence seems to witness for the inhibiting influence of the substitution of B by Si on the crystallization process.  相似文献   

13.
57Fe doped titanium oxide monocrystals, prepared by ion implantation at different temperatures and subsequent thermal treatment, were characterized by conversion electron Mössbauer spectrometry, synchrotron radiation x-ray diffraction and superconducting quantum interference device magnetometry. After implantation at room temperature Fe is present in divalent state. Upon annealing in high vacuum Fe2?+? is reduced to metallic Fe for the most part. After implantation at 623 K most iron is in metallic state. During annealing on air Fe is gradually oxidized from Fe2?+? to Fe3?+?. Depending on preparation conditions and thermal treatment the role of different nanosized secondary phases is discussed in terms of their influence on the magnetic properties of Fe:TiO2. α-Fe nanoparticles are found to be responsible for ferromagnetism observed in TiO2.  相似文献   

14.
The effects of layer thickness and thermal annealing on Curie temperature have been studied for CoPt ultrathin continuous layers in AlN/CoPt multilayer structures. It is found that there exists a critical thickness below which Curie temperature rapidly decreases due to the loss of spin-spin interactions in the vicinity of interface. After high temperature annealing, the in-plane lattice constant of CoPt film is increased and the exchange coupling parameter is decreased. Consequently, Curie temperatures decrease for some films with large thickness, compared with as-deposited state. Upon annealing at 600?°C, CoPt undergoes ordering transformation, which also contributes to the degradation of the Curie temperature. However, when the CoPt film thickness is below 2?nm, the Curie temperature is increased after annealing. Especially for 1?nm thick film, the Curie temperature is strikingly increased from 173?°C to 343?°C after annealing at 600?°C. This effect is attributed to the out-of-plane lattice deformation of CoPt thin layers in AlN/CoPt multilayer structures.  相似文献   

15.
NiFe2O4 nanoparticles have been synthesized by co-precipitation method at 145°C in N2 atmosphere using ethylene glycol as solvent and capping agent. This gives the promising synthesis route for nanoparticles at low temperature. The as-synthesized NiFe2O4 is subsequently heated at 400°C, 500°C, 700°C and 800°C. Crystallite size increases with the heat treatment temperature. The heat treatment temperature has direct effect on the electron paramagnetic resonance and intrinsic magnetic properties. The room temperature Mössbauer spectrum of the 800°C heated sample shows the two sextets pattern indicating that the sample is ferrimagnetic and Fe3?+? ions occupy both tetrahedral and octahedral sites of spinel structure.  相似文献   

16.
G. Vogler 《Annalen der Physik》1971,482(3):296-302
A Curie point shift in Mn? Zn? Fe-ferrites after sintering or annealing at small partial oxygen pressures between 10?1 and 10?3 Torr at 1200°C was measured. The effect is explained with the increasing number of Zn-ions on B-sites and Fe3?-ions on A-sites of the spinel lattice at high temperatures. Because of the small cation vacancy concentration at these partial oxygen pressures, the Zn-ions on B-sites cannot return on the A-sites during cooling and the Curie point is shifted to higher temperatures. The Curie point shift can be used to determine the stoichiometric state of Mn? Zn? Fe-ferrites, if the desaccommodation method and the determination of the active oxygen cannot be used.  相似文献   

17.
This work presents the results of the analysis of copiapite, formed from weathering and oxidation of pyrite in pyritic schist from Wie?ciszowice, Lower Silesia (Poland). The pure phase of copiapite was found in secondary minerals after pyrite and identified by optical microscopy, XRD and Mössbauer spectroscopy. In the analyzed copiapite major cations appear to be Fe2?+? and Fe3?+?. Some Fe3?+? is substituted by other cations, mainly Al3?+?. Al3?+? probably comes from leaching of chlorite from which hydrated sulphates of iron, mainly szomolnokite, form followed by hydrated sulphates fibroferrite, which is replaced by copiapite.  相似文献   

18.
The consequences of swift heavy ion (SHI) irradiation (Li3?+?, 50 MeV, fluence =?5 × 1013 ions/cm2) on the structural and microscopic magnetic properties of Y3?+?-substituted yttrium iron garnet (Y3?+?x Fe5???x O12, x = 0.0, 0.2 and 0.4) have been studied at 300 K. It is found that an additional YFeO3-phase observed along with bcc garnet phase, is completely removed for x = 0.2 composition while its percentage formation considerably reduces for x = 0.4 composition after irradiation. Similar effect has been observed for specimens sintered at 1,500°C. The SHI-induced ion beam mixing has been revealed through X-ray diffraction and Mössbauer spectroscopy.  相似文献   

19.
Room temperature 57Fe Mössbauer spectroscopy has been used to investigate the structural and oxidation state of Fe in tektites from different strewn fields. Spectra have been analyzed in terms of two quadrupole splitting distributions corresponding to Fe3?+? and Fe2?+?. All tektites show similar distribution of quadrupole splitting. Each distribution has one peak. The Fe2?+? sites show a narrow region of Mössbauer line shift (δ) and quadrupole splitting (ε), δ?= 1.02–1.10 mm/s and ε?= 0.85–1.00 mm/s relative to α-Fe. These values have been assigned to intermediate coordination between tetrahedral and octahedral. The Fe3?+? sites show wider regions of hyperfine parameters: δ?= 0.25–0.45 mm/s and ε?= 0.65–0.90 mm/s. The Fe3?+?/Fe2?+? ratio was found to be 0.05–0.15.  相似文献   

20.
It was suggested that Na–Mg carbonates might play a substantial role in mantle metasomatic processes through lowering melting temperatures of mantle peridotites. Taking into account that natrite, Na2CO3, eitelite, Na2Mg(CO3)2, and magnesite, MgCO3, have been recently reported from xenoliths of shallow mantle (110–115?km) origin, we performed experiments on phase relations in the system Na2CO3–MgCO3 at 3?GPa and 800–1250°C. We found that the subsolidus assemblages comprise the stability fields of Na-carbonate?+?eitelite and eitelite?+?magnesite with the transition boundary at 50?mol% Na2CO3. The Na-carbonate–eitelite eutectic was established at 900°C and 69?mol% Na2CO3. Eitelite melts incongruently to magnesite and a liquid containing about 55?mol% Na2CO3 at 925?±?25 °C. At 1050 °C, the liquid, coexisting with Na-carbonate, contains 86–88?mol% Na2CO3. Melting point of Na2CO3 was established at 1175?±?25 °C. The Na2CO3 content in the liquid coexisting with magnesite decreases to 31?mol% as temperature increases to 1250°C. According to our data, the Na- and Mg-rich carbonate melt, which is more alkaline than eitelite, can be stable at the P–T conditions of the shallow lithospheric mantle with thermal gradient of 45?mW/m2 corresponding to temperature of 900 °C at 3?GPa.  相似文献   

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