Fizička svojstva nanočestičnog kremenog gela punjenog s CdS i pripremljenog metodom otopina-gel

CdS/silica xerogel glasses were prepared via silica gels containing mixture solution of 0.2 M (CdCl2 and thiourea) with molar ratio 1:1. Doping the gels with this mixture solution and its heat treatment gave transparent yellow silica-gel glasses doped with CdS crystals. X-ray diffraction and transmission electron microscope make it possible to evaluate the nanoparticle size of the prepared samples. The nanoparticle size was dependent on the concentration of the dopant materials and the heating temperature. In the optical transmission spectra, the absorption edge exhibited a blue shift compared to that of the bulk CdS, and its energy shift was reciprocally proportional to the square of the radius. Thus the quantum-size effect could be found for the silica gel containing CdS prepared by the sol-gel process. The energy band gap shifted to higher energy for smaller nanoparticle size.Pripremili smo kserogel stakla CdS/kremen od kremenih gelova otopine 0.2M CdCl2 i tiouree s molarnim omjerom 1:1. Punjenje gelova tom otopinom i njihova toplinska obrada dali su prozirna žuta stakla s CdS kristalićima. Veličinu nanočestica u pripremljenim uzorcima odredili smo rendgenskom difrakcijom i prolaznom elektronskom mikroskopijom. Veličina nanočestica ovisi o koncentraciji punila i temperaturi pri toplinskoj obradi. Apsorpcijski rub optičkih prolaznih spektara pokazuje pomak prema plavom u odnosu na uzorke CdS, a energijski pomak je obrnuto proporcionalan kvadratu polumjera čestica. Tako se utvrdio kvantni učinak u kremenom gelu punjenom s CdS i pripremljenom metodom otopina-gel. Energijski se procjep povećava za manje veličine nanočestica

Fizička svojstva nanočestičnog kremenog gela punjenog s CdS i pripremljenog metodom otopina-gel

CdS/silica xerogel glasses were prepared via silica gels containing mixture solution of 0.2 M (CdCl2 and thiourea) with molar ratio 1:1. Doping the gels with this mixture solution and its heat treatment gave transparent yellow silica-gel glasses doped with CdS crystals. X-ray diffraction and transmission electron microscope make it possible to evaluate the nanoparticle size of the prepared samples. The nanoparticle size was dependent on the concentration of the dopant materials and the heating temperature. In the optical transmission spectra, the absorption edge exhibited a blue shift compared to that of the bulk CdS, and its energy shift was reciprocally proportional to the square of the radius. Thus the quantum-size effect could be found for the silica gel containing CdS prepared by the sol-gel process. The energy band gap shifted to higher energy for smaller nanoparticle size.Pripremili smo kserogel stakla CdS/kremen od kremenih gelova otopine 0.2M CdCl2 i tiouree s molarnim omjerom 1:1. Punjenje gelova tom otopinom i njihova toplinska obrada dali su prozirna žuta stakla s CdS kristalićima. Veličinu nanočestica u pripremljenim uzorcima odredili smo rendgenskom difrakcijom i prolaznom elektronskom mikroskopijom. Veličina nanočestica ovisi o koncentraciji punila i temperaturi pri toplinskoj obradi. Apsorpcijski rub optičkih prolaznih spektara pokazuje pomak prema plavom u odnosu na uzorke CdS, a energijski pomak je obrnuto proporcionalan kvadratu polumjera čestica. Tako se utvrdio kvantni učinak u kremenom gelu punjenom s CdS i pripremljenom metodom otopina-gel. Energijski se procjep povećava za manje veličine nanočestica

Proučavanje luminescencije uzbudom naviše u nanokristalima BaTiO3: Ho3+

Visible up-conversion emissions at 435, 545, 580, 675 and 690 nm and 437, 547, 575 and 675 nm have been obtained from BaTiO3 doped with 4 % Ho3+ ions in two different forms of the prepared samples, powder and thin film, under 808 nm laser diode excitation emissions. Combined with the energy level structure of Ho3+ ions and the kinetics of the visible emissions, the up-conversion mechanism has been analyzed and explained. The blue, green and red emissions of both samples have been attributed to the ground state-directed transition from 5F1, 5S2 and 5F5 states, respectively, which are populated through excited state absorption on 808 nm excitation. Nano-structure pure barium titanate and doped with different concentrations of Ho3+ ions in the form of powder and thin films have been prepared by so-gel technique, using barium acetate (Ba(CH3CHOO)2) and titanium isopropoxide (Ti((CH3)2CHO)4) as precursors. The thin films were prepared by spin-coating sol-gel method. The as-grown thin film and powders were found to be amorphous, which crystallized to the tetragonal phase after synthesization at 750 °C in air for 30 minutes. The crystallite size of thin film and powder samples both doped with 4 % Ho3+ ions, were found to be equal to 11 and 16 nm, respectively.Uzbudom laserskom diodom na 808 nm postigli smo emisije u vidljivom području na 435, 545, 580, 675 i 690 nm, te na 437, 547, 575 and 675 nm, u BaTiO3 punjenom s 4 % Ho3+ iona u uzorcima dvaju oblika, prahu i tankom sloju. Uzimajući u obzir stanja iona Ho3+ i kinetiku emisije fotona, analizirali smo i objasnili mehanizam uzbude naviše. Emisije oba uzorka u plavom, zelenom i crvenom području pripisuju se prijelazima u osnovno stanje sa stanja 5F1, 5S2 odn. 5F5 koja se pune apsorpcijom fotona 808 nm u višim stanjima Ho3+ iona. Metodom sol-gel pripremili smo nanostrukturni čist barijum titanat i barijum titanat punjen s dvjema koncentracijama Ho3+ iona, kao prah i kao tanke slojeve. Rabili smo barijum acetat (Ba(CH3CHOO)2) i titanijev izopropoksid (Ti((CH3)2CHO)4) za njihovu pripremu. Tanke smo slojeve dobivali centrifugiranjem sol-gela. Svježe pripremljeni tanki slojevi i prah su amorfni, ali se kristaliziraju zagrijavanjem na 750 ◦C u zraku tijekom 30 minuta. Veličina kristalita u tankom sloju i prahu, svaki punjen s 4 % Ho3+ iona, iznosi 11 odn. 16 nm

Proučavanje luminescencije uzbudom naviše u nanokristalima BaTiO3: Ho3+

Visible up-conversion emissions at 435, 545, 580, 675 and 690 nm and 437, 547, 575 and 675 nm have been obtained from BaTiO3 doped with 4 % Ho3+ ions in two different forms of the prepared samples, powder and thin film, under 808 nm laser diode excitation emissions. Combined with the energy level structure of Ho3+ ions and the kinetics of the visible emissions, the up-conversion mechanism has been analyzed and explained. The blue, green and red emissions of both samples have been attributed to the ground state-directed transition from 5F1, 5S2 and 5F5 states, respectively, which are populated through excited state absorption on 808 nm excitation. Nano-structure pure barium titanate and doped with different concentrations of Ho3+ ions in the form of powder and thin films have been prepared by so-gel technique, using barium acetate (Ba(CH3CHOO)2) and titanium isopropoxide (Ti((CH3)2CHO)4) as precursors. The thin films were prepared by spin-coating sol-gel method. The as-grown thin film and powders were found to be amorphous, which crystallized to the tetragonal phase after synthesization at 750 °C in air for 30 minutes. The crystallite size of thin film and powder samples both doped with 4 % Ho3+ ions, were found to be equal to 11 and 16 nm, respectively.Uzbudom laserskom diodom na 808 nm postigli smo emisije u vidljivom području na 435, 545, 580, 675 i 690 nm, te na 437, 547, 575 and 675 nm, u BaTiO3 punjenom s 4 % Ho3+ iona u uzorcima dvaju oblika, prahu i tankom sloju. Uzimajući u obzir stanja iona Ho3+ i kinetiku emisije fotona, analizirali smo i objasnili mehanizam uzbude naviše. Emisije oba uzorka u plavom, zelenom i crvenom području pripisuju se prijelazima u osnovno stanje sa stanja 5F1, 5S2 odn. 5F5 koja se pune apsorpcijom fotona 808 nm u višim stanjima Ho3+ iona. Metodom sol-gel pripremili smo nanostrukturni čist barijum titanat i barijum titanat punjen s dvjema koncentracijama Ho3+ iona, kao prah i kao tanke slojeve. Rabili smo barijum acetat (Ba(CH3CHOO)2) i titanijev izopropoksid (Ti((CH3)2CHO)4) za njihovu pripremu. Tanke smo slojeve dobivali centrifugiranjem sol-gela. Svježe pripremljeni tanki slojevi i prah su amorfni, ali se kristaliziraju zagrijavanjem na 750 ◦C u zraku tijekom 30 minuta. Veličina kristalita u tankom sloju i prahu, svaki punjen s 4 % Ho3+ iona, iznosi 11 odn. 16 nm

Strukturna i dielektrična svojstva nanostrukturnih prahova BaTiO3 punjenih ionima Eu3+ I pripremljenih sol-gel procesom

Nano-structure BaTiO3 powders doped with Eu3+ ions have been prepared by a sol-gel technique. X-ray diffraction (XRD) results indicate that BaTiO3 gel powders crystallize into tetragonal symmetry on heat treatment at 750 ◦C. Particle sizes as small as 3.5 nm were measured for pure BaTiO3 powders. The XRD data were confirmed by transmission electron microscope. Room-temperature luminescence spectra of BaTiO3:0.5% Eu3+, BaTiO3:1% Eu3+ and BaTiO3:2% Eu3+ powders have been measured. The luminescence spectra of prepared ultrafine powders are dominated by the 5D0 →7F2 transition in Eu3+, suggesting a strong distortion of the Eu3+ sites. The foreign ions are mainly accommodated in Ba2+ tetragonal sites, which are then distorted by the occurrence of different ionic charge of the two cations Ba2+ and Eu3+. The dielectric constant, ε, of BaTiO3, BaTiO3:0.5% Eu3+, BaTiO3:1% Eu3+ and BaTiO3:2% Eu3+ powders at frequency 100 Hz was found to be equal to 1000, 1211, 1455 and 1800, respectively. This high dielectric constant is believed to arise from the increase of the crystallite size, when increasing the concentration of Eu3+ ions. After annealing in argon at 400 ◦C for two hours, at 100 Hz, the dielectric constant of the pure sample was 625 and the AC resistivity also decreased. The room temperature (RT) AC resistivity of the samples depends on the concentration of Eu3+ ions in BaTiO3 powders, and was found to decrease as the concentration of Eu3+ ions increased.Pripremali smo sol-gel metodom nanostrukturne prahove BaTiO3 punjene Eu3+ ionima. Difrakcija X-zračenja (DXZ) pokazuje da se gel prahovi BaTiO3 kristaliziraju u tetragonalnoj simetriji zagrijavanjem na 750 ◦C. Utvrdili smo veličine zrna od samo 3.5 nm u čistom prahu BaTiO3. Podatke od DXZ potvrdili smo prolaznom elektronskom mikroskopijom. Mjerili smo fotoluminescentne spektre prahova BaTiO3:0.5% Eu3+, BaTiO3:1% Eu3+ i BaTiO3:2% Eu3+ na sobnoj temperaturi. U luminescentnim spektrima pripremljenih ultrafinih prahova prevladava prijelaz 5D0 →7F2 u Eu3+, što ukazuje na snažna izobličenja na mjestima Eu3+ iona. Ugrađeni se ioni Eu3+ uglavnom smještaju na tetragonalne položaje Ba2+, a velika razlika ionskih naboja dvaju kationa, Ba2+ i Eu3+, uzrokuje snažne promjene oko tog defekta. Dielektrične konstante, ε, prahova BaTiO3, BaTiO3:0.5% Eu3+, BaTiO3:1% Eu3+ i BaTiO3:2% Eu3+ na frekvenciji 100 Hz prema našim mjerenjima iznose 1000, 1211, 1455 odn. 1800. Smatramo da su tako velike vrijednosti dielektrične konstante posljedica povećanih veličina kristalita za veća punjenja ionima Eu3+. Nakon opuštanja u argonu na 400 ◦C tijekom dva sata, dielektrična konstanta čistog praha bila je 625, a otpornost se također smanjila. Izmjenična otpornost prahova BaTiO3 ovisi o punjenju ionima Eu3+ i nalazi se da se smanjuje kada se poveća sadržaj iona Eu3+

Strukturna i dielektrična svojstva nanostrukturnih prahova BaTiO3 punjenih ionima Eu3+ I pripremljenih sol-gel procesom

Nano-structure BaTiO3 powders doped with Eu3+ ions have been prepared by a sol-gel technique. X-ray diffraction (XRD) results indicate that BaTiO3 gel powders crystallize into tetragonal symmetry on heat treatment at 750 ◦C. Particle sizes as small as 3.5 nm were measured for pure BaTiO3 powders. The XRD data were confirmed by transmission electron microscope. Room-temperature luminescence spectra of BaTiO3:0.5% Eu3+, BaTiO3:1% Eu3+ and BaTiO3:2% Eu3+ powders have been measured. The luminescence spectra of prepared ultrafine powders are dominated by the 5D0 →7F2 transition in Eu3+, suggesting a strong distortion of the Eu3+ sites. The foreign ions are mainly accommodated in Ba2+ tetragonal sites, which are then distorted by the occurrence of different ionic charge of the two cations Ba2+ and Eu3+. The dielectric constant, ε, of BaTiO3, BaTiO3:0.5% Eu3+, BaTiO3:1% Eu3+ and BaTiO3:2% Eu3+ powders at frequency 100 Hz was found to be equal to 1000, 1211, 1455 and 1800, respectively. This high dielectric constant is believed to arise from the increase of the crystallite size, when increasing the concentration of Eu3+ ions. After annealing in argon at 400 ◦C for two hours, at 100 Hz, the dielectric constant of the pure sample was 625 and the AC resistivity also decreased. The room temperature (RT) AC resistivity of the samples depends on the concentration of Eu3+ ions in BaTiO3 powders, and was found to decrease as the concentration of Eu3+ ions increased.Pripremali smo sol-gel metodom nanostrukturne prahove BaTiO3 punjene Eu3+ ionima. Difrakcija X-zračenja (DXZ) pokazuje da se gel prahovi BaTiO3 kristaliziraju u tetragonalnoj simetriji zagrijavanjem na 750 ◦C. Utvrdili smo veličine zrna od samo 3.5 nm u čistom prahu BaTiO3. Podatke od DXZ potvrdili smo prolaznom elektronskom mikroskopijom. Mjerili smo fotoluminescentne spektre prahova BaTiO3:0.5% Eu3+, BaTiO3:1% Eu3+ i BaTiO3:2% Eu3+ na sobnoj temperaturi. U luminescentnim spektrima pripremljenih ultrafinih prahova prevladava prijelaz 5D0 →7F2 u Eu3+, što ukazuje na snažna izobličenja na mjestima Eu3+ iona. Ugrađeni se ioni Eu3+ uglavnom smještaju na tetragonalne položaje Ba2+, a velika razlika ionskih naboja dvaju kationa, Ba2+ i Eu3+, uzrokuje snažne promjene oko tog defekta. Dielektrične konstante, ε, prahova BaTiO3, BaTiO3:0.5% Eu3+, BaTiO3:1% Eu3+ i BaTiO3:2% Eu3+ na frekvenciji 100 Hz prema našim mjerenjima iznose 1000, 1211, 1455 odn. 1800. Smatramo da su tako velike vrijednosti dielektrične konstante posljedica povećanih veličina kristalita za veća punjenja ionima Eu3+. Nakon opuštanja u argonu na 400 ◦C tijekom dva sata, dielektrična konstanta čistog praha bila je 625, a otpornost se također smanjila. Izmjenična otpornost prahova BaTiO3 ovisi o punjenju ionima Eu3+ i nalazi se da se smanjuje kada se poveća sadržaj iona Eu3+

Ramanovi i fotoluminescentni spektri čistih i kositrom obogaćenih tankih slojeva CdS pripremljenih prskanjem i pirolizom

Thin films of CdS, pure and enriched with different concentrations of tin up to 6%, were prepared by the spray pyrolysis technique. All samples were prepared at the deposition temperature of 420 ◦C. The XRD diagnostic data of the investigated samples revealed the polycrystalline nature of the as-deposited samples. The main characteristic peaks of CdS appeared in both pure and enriched films prepared by all used methods. The enrichment of Sn has no effect on positions of the characteristic peaks. The observed effect of Sn enrichment is the change in peak broadening which increases with the increase of Sn concentration. The thickness values ranged from 0.65 up to 1.15 µm. The samples of pure CdS show a sharp absorption edge at about 2.43 eV. The absorption coefficient α of the investigated samples was calculated from transmission and reflection spectra. Photoluminescence measurements show red emission band of the as-deposited samples, which was quenched by Sn incorporation. This band is ascribed to the excess of Cd which was checked by the energy dispersive X-ray (EDX) spectrometry. Raman spectra of samples with different concentrations of Sn were studied. They show remarkable increase of intensity when increasing the film thickness and decreasing the Sn concentration.Metodom prskanja i pirolize pripremali smo čiste i do 6% kositrom obogaćene tanke slojeve CdS. Sve uzorke smo pripremali na temperaturi polaganja od 420 ◦C. XRD spektri ispitivanih uzoraka pokazuju polikristaliničnu strukturu. Glavni karakteristični vrhovi CdS vide se i u čistim i u obogaćenim uzorcima pripremljenim primijenjenim metodama. Obogaćenje kositrom nema utjecaja na položaje karakterističnih vrhova. Međutim, javlja se proširenje vrhova koje se povećava pri povećanim koncentracijama kositra. Izmjerene i izračunate debljine slojeva su u skladu. Debljine slojeva bile su između 0.65 i 1.15 µm. Uzorci CdS pokazuju oštar apsorpcijski rub na oko 2.43 eV. Apsorpcijske koeficijente α ispitivanih uzoraka smo izveli iz transmisijskih i refleksijskih spektara. Mjerenja fotoluminescencije pokazuju crvenu emisijsku vrpcu koja trne dodavanjem kositra. Ta se vrpca tumači viškom Cd što smo potvrdili disperzivnom rendgenskom spektrometrijom (EDX). Proučavali smo i Ramanove spektre uzoraka s raznim koncentracijama kositra. Oni pokazuju snažan porast intenziteta za slojeve veće debljine i manje koncentracije kositra

Ramanovi i fotoluminescentni spektri čistih i kositrom obogaćenih tankih slojeva CdS pripremljenih prskanjem i pirolizom

Thin films of CdS, pure and enriched with different concentrations of tin up to 6%, were prepared by the spray pyrolysis technique. All samples were prepared at the deposition temperature of 420 ◦C. The XRD diagnostic data of the investigated samples revealed the polycrystalline nature of the as-deposited samples. The main characteristic peaks of CdS appeared in both pure and enriched films prepared by all used methods. The enrichment of Sn has no effect on positions of the characteristic peaks. The observed effect of Sn enrichment is the change in peak broadening which increases with the increase of Sn concentration. The thickness values ranged from 0.65 up to 1.15 µm. The samples of pure CdS show a sharp absorption edge at about 2.43 eV. The absorption coefficient α of the investigated samples was calculated from transmission and reflection spectra. Photoluminescence measurements show red emission band of the as-deposited samples, which was quenched by Sn incorporation. This band is ascribed to the excess of Cd which was checked by the energy dispersive X-ray (EDX) spectrometry. Raman spectra of samples with different concentrations of Sn were studied. They show remarkable increase of intensity when increasing the film thickness and decreasing the Sn concentration.Metodom prskanja i pirolize pripremali smo čiste i do 6% kositrom obogaćene tanke slojeve CdS. Sve uzorke smo pripremali na temperaturi polaganja od 420 ◦C. XRD spektri ispitivanih uzoraka pokazuju polikristaliničnu strukturu. Glavni karakteristični vrhovi CdS vide se i u čistim i u obogaćenim uzorcima pripremljenim primijenjenim metodama. Obogaćenje kositrom nema utjecaja na položaje karakterističnih vrhova. Međutim, javlja se proširenje vrhova koje se povećava pri povećanim koncentracijama kositra. Izmjerene i izračunate debljine slojeva su u skladu. Debljine slojeva bile su između 0.65 i 1.15 µm. Uzorci CdS pokazuju oštar apsorpcijski rub na oko 2.43 eV. Apsorpcijske koeficijente α ispitivanih uzoraka smo izveli iz transmisijskih i refleksijskih spektara. Mjerenja fotoluminescencije pokazuju crvenu emisijsku vrpcu koja trne dodavanjem kositra. Ta se vrpca tumači viškom Cd što smo potvrdili disperzivnom rendgenskom spektrometrijom (EDX). Proučavali smo i Ramanove spektre uzoraka s raznim koncentracijama kositra. Oni pokazuju snažan porast intenziteta za slojeve veće debljine i manje koncentracije kositra

Sol–gel-derived photonic structures handling erbium ions luminescence

The sol–gel technique is a very flexible, relatively simple, and low-cost method to fabricate many different innovative photonic structures characterized by specific functionalities. During synthesis, starting from the molecular level, compounds or composites with well controlled composition can be obtained as thin films, powders or monoliths. These materials can be used to prepare such structures as waveguides, photonic crystals, coatings, and bulk glasses including spheres, rings and other geometries exploited in optical resonators fabrication. This article presents some results obtained by the authors in the field of the sol–gel-derived photonic structures. To emphasise the scientific and technological interest in this kind of systems and the versatility of the sol–gel route, the glass-based nano and micrometer scale range systems are discussed. Particularly, the following systems are described: silica–hafnia glass and glass–ceramic planar waveguides, nanosized tetraphosphates, and silica colloidal crystals. The attention is focused on the spectroscopic properties of Er3+-activated materials that due to the light emission can be used in the integrated optics area covering application in sensing, biomedical diagnostic, energy conversion, telecommunication, lighting, and photon management