RO138020A2 - Pbs-doped oxide films with optical properties for temperature sensors and process for synthesis thereof - Google Patents
Pbs-doped oxide films with optical properties for temperature sensors and process for synthesis thereof Download PDFInfo
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- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 7
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract 3
- 238000000151 deposition Methods 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 14
- 239000000377 silicon dioxide Substances 0.000 abstract description 7
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 6
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- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 229910052681 coesite Inorganic materials 0.000 abstract 2
- 229910052593 corundum Inorganic materials 0.000 abstract 2
- 229910052906 cristobalite Inorganic materials 0.000 abstract 2
- 229910052682 stishovite Inorganic materials 0.000 abstract 2
- 229910052905 tridymite Inorganic materials 0.000 abstract 2
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 2
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 17
- 239000002096 quantum dot Substances 0.000 description 17
- XCAUINMIESBTBL-UHFFFAOYSA-N lead(ii) sulfide Chemical compound [Pb]=S XCAUINMIESBTBL-UHFFFAOYSA-N 0.000 description 12
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
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- 238000003980 solgel method Methods 0.000 description 5
- YBNMDCCMCLUHBL-UHFFFAOYSA-N (2,5-dioxopyrrolidin-1-yl) 4-pyren-1-ylbutanoate Chemical compound C=1C=C(C2=C34)C=CC3=CC=CC4=CC=C2C=1CCCC(=O)ON1C(=O)CCC1=O YBNMDCCMCLUHBL-UHFFFAOYSA-N 0.000 description 4
- 229910003849 O-Si Inorganic materials 0.000 description 4
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- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 230000001419 dependent effect Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
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- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- 229910008051 Si-OH Inorganic materials 0.000 description 2
- 229910006358 Si—OH Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
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- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
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- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 1
- 240000002769 Morchella esculenta Species 0.000 description 1
- 235000002779 Morchella esculenta Nutrition 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
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- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
ZICIUL BB STAT PiNTRU MVINTM W M^RCITHE SAYING BB STAT PiNTRU MVINTM W M^RCI
Cerere de brevet de InvențieInvention patent application
DESCRIERE INVENȚIE depozitDESCRIPTION OF THE DEPOSIT
Invenția se referă la produsele de tip filme oxidice dopate cu nanoparticule (puncte cuantice) semiconductoare de PbS (sulfură de plumb), având aplicație în dispozitivele senzori de temperatură și la procedeul de obținere a acestor filme. în scopul preparării acestor filme oxidice, se aplică metoda sol-gel, tehnica de depunere pe substrate rotative de sticlă și, respectiv, de oxid de indiu dopat cu oxid de staniu (ITO), depuse pe sticlă. Această metodă utilizează materii prime de tip săruri organo-metalice, esteri organici, săruri anorganice. Acestea introduc oxidul de aluminiu, dioxidul de siliciu și pentaoxidul de fosfor ca formatori de rețea vitroasă precum și PbS ca dopant. Alcoolul etilic este utilizat ca mediu de reacție iar monoetanol amina este un reactiv utilizat pentru accelerarea procesului de gelifiere (hidroliză și condensare). PbS se prezintă sub formă de nanoparticule cu dimensiunea cuprinsă între 7-7,5 nm, acoperite cu acid oleic și dispersate în toluen, având fotoluminescența la aproximativ 1400 nm, prin excitare la 800 nm. Reactanții se introduc în cantitățile corespunzătoare compozițiilor prestabilite, în vederea desfășurării procesului de gelifiere a amestecului de precursori. Metoda sol-gel de preparare a filmelor oxidice dopate cu nanoparticule de PbS constă în omogenizarea mecanică a reactanților în soluție, urmată de efectuarea celor 20 de depuneri ale soluției pe substrate rotative si tratarea termică a fiecărei depuneri, la temperatura de 100°C, în vederea uscării materialului depus, pentru eliminarea apei și a alcoolului etilic. Filmele uscate sunt tratate termic la temperatura de 200°C, în vid, în vederea descompunerii compușilor organici intermediari ai siliciului, fosforului si aluminiului și formării rețelei vitroase mixte AhOj-SiCh-PzOs. Acest tratament termic permite desfășurarea reacțiilor chimice de descompunere a produșilor de hidroliză și condensare cu formarea rețelei oxidice vitroase, rețea care include sulfura de plumb ca dopant. Compoziția chimică, durata de gelifiere și valoarea pH a amestecului de reactanți precursori, alături de viteza de rotație a substratului și de numărul de straturi depuse, reprezintă parametri care influențează procesul de gelifiere. Metoda de sinteză sol-gel are ca scop prepararea unor filme omogene din punct de vedere chimic si uniforme din punct de vedere a grosimii. în felul acesta, metoda sol-gel permite obținerea unor filme cu costuri relativ scăzute, comparativ cu alte metode de sinteză a filmelor dopate precum și procesarea soluției precursoare la temperaturi relativ scăzute. Totodată, această metodă permite obținerea unor filme dopate cu sulfură de plumb cu proprietăți optice de interes, având aplicații în domeniul senzorilor de temperatură pe bază de fotoluminescență.The invention refers to oxide film products doped with PbS (lead sulphide) semiconductor nanoparticles (quantum dots), having application in temperature sensor devices and to the process of obtaining these films. in order to prepare these oxide films, the sol-gel method is applied, the deposition technique on rotating glass substrates and, respectively, of indium oxide doped with tin oxide (ITO), deposited on glass. This method uses raw materials such as organo-metallic salts, organic esters, inorganic salts. They introduce aluminum oxide, silicon dioxide and phosphorus pentaoxide as glass network formers as well as PbS as a dopant. Ethyl alcohol is used as a reaction medium and monoethanolamine is a reagent used to accelerate the gelation process (hydrolysis and condensation). PbS is presented in the form of nanoparticles with a size between 7-7.5 nm, coated with oleic acid and dispersed in toluene, having photoluminescence at approximately 1400 nm, by excitation at 800 nm. The reactants are introduced in the quantities corresponding to the predetermined compositions, in order to carry out the gelation process of the precursor mixture. The sol-gel method for preparing oxide films doped with PbS nanoparticles consists in the mechanical homogenization of the reactants in the solution, followed by the 20 depositions of the solution on rotating substrates and the thermal treatment of each deposition, at a temperature of 100°C, in to dry the deposited material, to remove water and ethyl alcohol. The dry films are thermally treated at a temperature of 200°C, in a vacuum, in order to decompose the intermediate organic compounds of silicon, phosphorus and aluminum and to form the mixed vitreous network AhOj-SiCh-PzOs. This thermal treatment allows the chemical reactions of the decomposition of the hydrolysis and condensation products to take place with the formation of the vitreous oxide network, a network that includes lead sulphide as a dopant. The chemical composition, the gelation time and the pH value of the mixture of precursor reactants, along with the rotation speed of the substrate and the number of deposited layers, are parameters that influence the gelation process. The sol-gel synthesis method aims to prepare films that are chemically homogeneous and uniform in thickness. In this way, the sol-gel method allows obtaining films with relatively low costs, compared to other methods of synthesis of doped films as well as the processing of the precursor solution at relatively low temperatures. At the same time, this method allows obtaining films doped with lead sulphide with interesting optical properties, having applications in the field of temperature sensors based on photoluminescence.
Situația actuală la nivel internaționalThe current situation at the international level
Nanoparticulele coloidale semiconductoare (puncte cuantice) au atras un interes științific și tehnologic mărit, în ultimele trei decenii, datorită ajustării proprietăților lor optoelectronice prin variația dimensiunii și compoziției. Cu toate acestea, dimensiunea la scară nanometrică aduce un raport mare intre suprafața și volumul nanoparticulelor, în care suprafețele nanoparticulelor prezintă o influență importantă asupra stabilității chimice și asupra proprietăților fizice ale materialului semiconductor [1]. Sulfura de plumb (PbS) este un material semiconductor având banda de energie interzisă îngustă, de aproximativ 0,4 eV la 300 K și o rază a excitonului Bohr relativ mare, de 18 nm, ceea ce face ca PbS să fie foarte potrivită pentru aplicațiile de detecție în infraroșu. Un studiu recent bazat pe nanoparticulele de PbS sintetizate prin metoda chimică coloidală a fost raportat în [2], în legătură cu influența temperaturii (10 K-300 K) și a puterii de excitație asupra caracteristicilor fotoluminescenței. O deplasare a maximului de fotoluminescență spre domeniul albastru al spectrului vizibil a fost observată odată cu creșterea temperaturii, împreună cu o lărgire a benzilor de fotoluminescență, datorită interacțiunilor purtătorilor de sarcină cu fononii. Rezultatele recente arată că nanoparticulele de PbS constituie un material fotonic remarcabil în domeniul nanotehnologiei, cu aplicații în dispozitivele electronice și fotonice de generație nouă, datorită efectului de confinare cuantica dependent de dimensiunea nanoparticulelor. Nanoparticulele de PbS prezintă fotoluminescență în domeniul infraroșu, dependentă de dimensiunea acestora. Au fost raportate soluții de nanoparticule de PbS și filme subțiri, avand fotoluminescență îngustă, randament cuantic ridicat, foto-stabilitate remarcabilă și fotoluminiscență în intervalul 1000-1650 nm prin excitare la 785 nm [3]. Au fost raportate puncte cuantice IV-VI (PbS, PbSe) cu dimensiunea de 2,7-7,6 nm, fotoluminiscență în intervalul 800-2000 nm și cinetică de dezintegrare în intervalul de timp de 0,01-10 μ8 [4] precum și fotoluminiscență a nanoparticulelor IV-VI în intervalul 800-2000 nm, proprietăți de fotoluminiscență cinetică între 0,8 și 1,7 pm, rezoluție de 3 ns și dimensiunea nanoparticulelor de PbS între 3,4-8,4 nm [5]. Posibilitatea de a adapta proprietățile optice prin modificarea dimensiunii nanoparticulelor oferă acestor materiale potențialul de a rezolva multe dintre cerințele senzorilor de temperatură pe bază de fotoluminiscență. Au fost raportate studii referitoare la punctele cuantice de PbS în oxid de grafenă și oxid de grafenă redusă [7]; fotoluminiscență nanoparticulelor de PbS în intervalul de temperatură 4-300 K, domeniul de fotoluminescență 1000-1200 nm, colectată prin excitare la 514 nm [8]; emisia punctelor cuantice de PbS cu dimensiunea de 3-6,5 nm, în domeniul 800-1000 nm și în intervalul de temperatură de 100-300 K [9] și senzori de temperatură fotoluminescenți cu fibră optică și puncte cuantice [10]. O eficiență cuantică mai mare datorită creșterii puterii oscilatorului oferă punctelor cuantice potențialul de a rivaliza cu ionii de pământuri rare utilizați în mod tradițional ca centri optic activi pentru detecția termică. O etapă către dezvoltarea dispozitivelor de opto-detecție, având costuri reduse, constă în imobilizarea punctelor cuantice în structuri solide. Aceste matrici gazdă, transparente optic, care conțin puncte cuantice de PbS, sunt necesare pentru aplicațiile de opto-detecție, prin încorporarea punctelor cuantice în matricea organică [11]. A fost raportată recent, emisia dependentă de temperatură a nanoparticulelor de PbS, deschizând astfel noi posibilități pentru dispozitivele optice de detecție a temperaturii, pe baza fotoluminiscenței între 850-950 nm și în domeniul de temperatură de 10-310 K, dimensiunea punctelor cunatice fiind de aproximativ 2,5 nm [12], O metodă de sinteză mai ușor de abordat pentru a obține nanocompozite pe bază de PbS, acoperite cu silice, cu dimensiuni ajustabile și proprietăți optice, a fost raportată în [13], în care, nanoparticulele de PbS au fost încorporate într-o matrice silicatică, având fotoluminiscență la 440 nm și 605 nm. Proprietățile optice dependente de dimensiune, ale punctelor cuantice de PbS, au fost investigate prin combinarea spectrelor de absorbție cu analiza elementală detaliată a soluțiilor de puncte cuantice [14], Dependența fotoluminiscenței de dimensiunea nanoparticulelor de PbS înglobate într-o sticlă silicatică complexă, a fost evidențiată pe baza stărilor de capcană electroni goluri ale punctelor cuantice care interacționează cu defectele de la interfața dintre punctele cuantice de PbS și rețeaua de sticlă [15]. Au fost prezentate, de asemenea, proprietățile microstructurale și optice ale senzorilor pe bază de puncte cuantice de PbS și detecția în infraroșu pentru aplicații optice și de bio-detecție [16]. Fotodetectorii pe bază de nanoparticule de PbS care operează în domeniul NIR (infraroșu apropiat) au fost studiați recent, cuprinzând o mare varietate de aplicații, inclusiv comunicații prin fibră optică, spectroscopie, imagistică, securitate, teledetecție și metrologie, cu aplicabilitate în domenii precum inspecția alimentară, agricultură, farmaceutică și biologie. Datorită confinării cuantice puternice a nanoparticulelor semiconductoare, acestea prezintă interacțiuni cu radiația luminoasă, oferind proprietăți optice unice, cum ar fi absorbția și emisia optică intense în dependență de dimensiunea punctelor cuantice. Din aceste motive, punctele cuantice au aplicații în dispozitive optoelectronice, inclusiv diode emițătoare de lumină, lasere, celule solare și fotodetectori [17-19]. Filmele pe bază de PbS au fost preparate prin diferite tehnici precum depunere chimică [20], piroliza prin pulverizare [21], depunere în baie chimică [2228], electrodepunere [29], depunere chimică foto-accelerată [30], încălzire cu microunde [31,32] și metoda de acoperire prin depunere pe substrat rotativ [33]. Punctele cuantice de PbSe/PbS de tip miez/inveliș de dimensiuni mici au fost investigate de Yanover et al. [34],Semiconducting colloidal nanoparticles (quantum dots) have attracted increased scientific and technological interest in the last three decades due to the tuning of their optoelectronic properties by varying their size and composition. However, the nanoscale size brings a large ratio between the surface and volume of the nanoparticles, where the surfaces of the nanoparticles have an important influence on the chemical stability and on the physical properties of the semiconductor material [1]. Lead sulfide (PbS) is a semiconductor material with a narrow band gap of about 0.4 eV at 300 K and a relatively large exciton Bohr radius of 18 nm, making PbS well suited for applications infrared detection. A recent study based on PbS nanoparticles synthesized by the colloidal chemical method was reported in [2], in relation to the influence of temperature (10 K-300 K) and excitation power on the photoluminescence characteristics. A shift of the photoluminescence maximum towards the blue region of the visible spectrum was observed with increasing temperature, together with a broadening of the photoluminescence bands, due to interactions of charge carriers with phonons. Recent results show that PbS nanoparticles constitute an outstanding photonic material in the field of nanotechnology, with applications in new generation electronic and photonic devices, due to the nanoparticle size-dependent quantum confinement effect. PbS nanoparticles exhibit size-dependent infrared photoluminescence. PbS nanoparticle solutions and thin films have been reported to have narrow photoluminescence, high quantum yield, remarkable photostability, and photoluminescence in the range of 1000–1650 nm upon excitation at 785 nm [3]. IV-VI quantum dots (PbS, PbSe) with size of 2.7-7.6 nm, photoluminescence in the range of 800-2000 nm and decay kinetics in the time range of 0.01-10 μ8 have been reported [4] as well as IV-VI nanoparticle photoluminescence in the 800-2000 nm range, kinetic photoluminescence properties between 0.8 and 1.7 pm, 3 ns resolution, and PbS nanoparticle size between 3.4-8.4 nm [5] . The ability to tailor the optical properties by changing the size of the nanoparticles gives these materials the potential to solve many of the requirements of photoluminescence-based temperature sensors. Studies on PbS quantum dots in graphene oxide and reduced graphene oxide have been reported [7]; photoluminescence of PbS nanoparticles in the temperature range 4-300 K, photoluminescence range 1000-1200 nm, collected by excitation at 514 nm [8]; emission of 3-6.5 nm PbS quantum dots in the 800-1000 nm range and 100-300 K temperature range [9] and photoluminescent temperature sensors with optical fiber and quantum dots [10]. Higher quantum efficiency due to increased oscillator strength gives quantum dots the potential to rival rare earth ions traditionally used as optically active centers for thermal sensing. One step towards the development of low-cost opto-detection devices is the immobilization of quantum dots in solid structures. These optically transparent host matrices containing PbS quantum dots are needed for opto-sensing applications by incorporating the quantum dots into the organic matrix [11]. Recently, the temperature-dependent emission of PbS nanoparticles has been reported, thus opening new possibilities for optical temperature detection devices, based on photoluminescence between 850-950 nm and in the temperature range of 10-310 K, the size of the cunatic points being about 2.5 nm [12], A more approachable synthesis method to obtain silica-coated PbS-based nanocomposites with tunable size and optical properties was reported in [13], where nanoparticles of PbS were embedded in a silicate matrix, having photoluminescence at 440 nm and 605 nm. The size-dependent optical properties of PbS quantum dots were investigated by combining absorption spectra with detailed elemental analysis of quantum dot solutions [14], The size dependence of photoluminescence of PbS nanoparticles embedded in a complex silicate glass was highlighted based on electron-hole trap states of quantum dots interacting with defects at the interface between the PbS quantum dots and the glass lattice [15]. The microstructural and optical properties of PbS quantum dot-based sensors and infrared detection for optical and bio-sensing applications have also been presented [16]. Photodetectors based on PbS nanoparticles operating in the NIR (near-infrared) range have recently been studied, encompassing a wide variety of applications, including fiber optic communications, spectroscopy, imaging, security, remote sensing, and metrology, with applicability in areas such as inspection food, agriculture, pharmaceutical and biology. Due to the strong quantum confinement of semiconductor nanoparticles, they exhibit interactions with light radiation, providing unique optical properties such as intense optical absorption and emission depending on the quantum dot size. For these reasons, quantum dots have applications in optoelectronic devices, including light-emitting diodes, lasers, solar cells, and photodetectors [17-19]. PbS-based films have been prepared by various techniques such as chemical deposition [20], spray pyrolysis [21], chemical bath deposition [2228], electrodeposition [29], photo-accelerated chemical deposition [30], microwave heating [31,32] and spin coating method [33]. Small-sized core/shell PbSe/PbS quantum dots were investigated by Yanover et al. [34],
iand
Astfel, diametrul miezului variază între 2-2,5 nm, diametrul carcasei între 0,5-1 nm și fotoluminescența apare la aproximativ 0,15 eV. Recent, punctele cuantice de dimensiuni mici pe bază de semiconductori PbSe/PbS cu structură miez/inveliș au fost sintetizate printr-o metodă de chimie umedă. Proprietățile lor electronice au fost determinate prin compararea calculelor teoretice cu măsurători de undă continuă și fotoluminiscență la diferite temperaturi [35]. A fost studiată influența tensiunilor la interfețe asupra proprietăților optice ale punctelor cuantice de PbSe/PbS. Profilul de deformare derivat a fost încorporat într-un calcul al structurii de benzi pentru a evalua influența asupra marginilor benzii electronice ale punctelor cuantice miez/înveliș [36].Thus, the core diameter varies between 2-2.5 nm, the shell diameter between 0.5-1 nm and photoluminescence occurs at about 0.15 eV. Recently, small size quantum dots based on PbSe/PbS semiconductors with core/shell structure have been synthesized by a wet chemistry method. Their electronic properties were determined by comparing theoretical calculations with continuous wave and photoluminescence measurements at different temperatures [35]. The influence of interfacial stresses on the optical properties of PbSe/PbS quantum dots was studied. The derived strain profile was incorporated into a band structure calculation to assess the influence on the electronic band edges of core/shell quantum dots [36].
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Descrierea generală a invențieiGeneral description of the invention
Filmele oxidice dopate cu puncte cuantice (nanoparticule) de sulfură de plumb (PbS), sintetizate prin metoda sol-gel, tehnica de depunere pe substrate rotative, aparțin sistemului compozițional 40(A1203-Si02-P205)-60PbS (% gravimetrice) și au fost depuse pe substrate de sticla și ITO, câte 20 de depuneri pe fiecare substrat. Au fost utilizați următorii reactivi chimici (puritate analitică) ca precursori ai oxizilor care se formează în materialul final: AcAcAlacetilacetonat de aluminiu (C15H21O6AI) precursor al oxidului de aluminiu (AI2O3), TEOStetraetilortosilicat ((Si(OC2Hs)4) precursor al dioxidului de siliciu (S1O2) și TEP-trietilfosfat (C6H15O4P) precursor al pentaoxidului de fosfor (P2O5). De asemenea, au mai fost utilizați alți reactivi chimici: EtOH-alcool etilic (C2H5OH) în calitate de mediu de reacție și MEA-monoetanolamina (C2H7NO), în calitate de catalizator bazic al reacțiilor de hidroliză și condensare, accelerând, astfel, procesul de gelifiere a amestecului de reactanți. In calitate de dopant, a fost utilizată PbS sub forma de nanoparticule acoperite cu acid oleic și dispersate în toluen, concentrație 10 mg/mL. Precursorii și ceilalți reactanți au fost dozați astfel încât, în materialul final obținut, să se realizeze următoarele rapoarte molare: SiO2/P2O5=l,3; SiO2/Al2O3=7,65; Ρ2Θ5/Α12θ3=6,08; SiO2/EtOH=2,6xl0-4; MEA/SiO2=l,02. Amestecul de precursori a fost omogenizat mecanic timp de 2 ore cu ajutorul unui agitator magnetic, apoi au fost efectuate cele 20 de depuneri pe substrate rotative de sticlă și, respectiv, de ITO. Viteza de rotație a fost cuprinsă între 2000-3000 rpm, fiecare depunere a durat 20 s, urmată de tratamentul termic pe plita electrică, la temperatura de 100°C, timp de 2 min, în scopul eliminării apei și a alcoolului etilic. Filmele astfel obținute, au fost tratate termic la 200°C, în etuva electrică, în vid, în vederea descompunerii compușilor organici intermediari ai Al, Si si P, cu formarea rețelei mixte AI2O3-S1O2-P2O5. Matricea vitroasă în care este înglobat dopantul, este stabilă chimic și termic, având o compoziție chimică adecvată pentru a asigura protecția față de oxidare a PbS, permițând fotoluminescența acesteia în domeniul infraroșu apropiat.The oxide films doped with quantum dots (nanoparticles) of lead sulfide (PbS), synthesized by the sol-gel method, the deposition technique on rotating substrates, belong to the compositional system 40(A1203-SiO2-P205)-60PbS (gravimetric %) and have were deposited on glass and ITO substrates, 20 depositions on each substrate. The following chemical reagents (analytical purity) were used as precursors of the oxides that form in the final material: Aluminum AcAcAlacetylacetonate (C15H21O6AI) precursor of aluminum oxide (AI2O3), TEOStetraethylorthosilicate ((Si(OC2Hs)4) precursor of silicon dioxide (S1O2) and TEP-triethylphosphate (C6H15O4P) precursor of phosphorus pentaoxide (P2O5). Other chemical reagents were also used: EtOH-ethyl alcohol (C2H5OH) as reaction medium and MEA-monoethanolamine (C2H7NO). , as the basic catalyst of the hydrolysis and condensation reactions, thus accelerating the gelation process of the reactant mixture. As a dopant, PbS was used in the form of nanoparticles coated with oleic acid and dispersed in toluene, concentration 10 mg /mL. The precursors and the other reactants were dosed so that, in the final material obtained, the following molar ratios were achieved: SiO 2 /Al 2 O3 = 7.65; Ρ 2 Θ 5 /Α12θ3 =6.08; SiO 2 /EtOH=2.6xl0-4 ; MEA/SiO 2 =1.02. The precursor mixture was mechanically homogenized for 2 h using a magnetic stirrer, then the 20 depositions were performed on rotating glass and ITO substrates, respectively. The rotation speed was between 2000-3000 rpm, each deposition lasted 20 s, followed by heat treatment on the electric plate, at a temperature of 100°C, for 2 min, in order to eliminate water and ethyl alcohol. The films thus obtained were thermally treated at 200°C, in an electric oven, in a vacuum, in order to decompose the intermediate organic compounds of Al, Si and P, with the formation of the mixed network AI2O3-S1O2-P2O5. The vitreous matrix in which the dopant is embedded is chemically and thermally stable, having an appropriate chemical composition to ensure protection against oxidation of PbS, allowing its photoluminescence in the near-infrared range.
Exemple de aplicare a invenției:Examples of application of the invention:
Exemplul 1Example 1
Compoziția gravimetrică nominală a filmului dopat cu PbS (20 de depuneri succesive) pe substrat de sticla, este: 2,97 % AI2O3,13,39 % S1O2, 25,21 % P2O5, 58,41 % PbS (Cod PbSl).The nominal gravimetric composition of the PbS-doped film (20 successive depositions) on a glass substrate is: 2.97% AI2O3, 13.39% S1O2, 25.21% P2O5, 58.41% PbS (Code PbSl).
în tabelul 1 se prezintă volumele/cantitățile de reactanți utilizați pentru prepararea amestecului precursor, depus pe substrat rotativ de sticlă (PbSl).Table 1 shows the volumes/quantities of reactants used for the preparation of the precursor mixture, deposited on a rotating glass substrate (PbSl).
Tabelul 1. Volumele/cantitățile de reactanți utilizați la prepararea amestecului precursor, depus pe substrat rotativ de sticlă (PbSl).Table 1. Volumes/amounts of reactants used in the preparation of the precursor mixture, deposited on a rotating glass substrate (PbSl).
Etapele procesului de sinteza a filmului oxidic dopat cu PbS sunt: (i) Omogenizarea soluției conținând amestecul de precursori (Tabelul 1) la temperatura camerei, timp de 2 ore, utilizând un agitator magnetic; (ii) efectuarea celor 20 de depuneri succesive, pe substrat de sticlă, fiecare depunere a durat 20 s, viteza de rotație fiind de 2000 rpm; (iii) tratamentul termic (uscare) al fiecărei depuneri, la temperatura de 100°C, timp de 2 min, în vederea eliminării apei și a alcoolului etilic; (iv) filmul multistrat obținut, a fost tratament termic în etuvă, în vid, la temperatura de 200°C, în vederea descompunerii compușilor organici intermediari ai Al, Si si P, cu formarea rețelei mixte AI2O3-S1O2-P2O5: (v) caracterizarea optică a filmului obținut, privind transmisia in domeniul UV-Vis-NIR si fotoluminescența în domeniul NIR.The steps of the synthesis process of the oxide film doped with PbS are: (i) Homogenization of the solution containing the mixture of precursors (Table 1) at room temperature, for 2 hours, using a magnetic stirrer; (ii) performing the 20 successive depositions, on a glass substrate, each deposition lasted 20 s, the rotation speed being 2000 rpm; (iii) thermal treatment (drying) of each deposition, at a temperature of 100°C, for 2 min, in order to eliminate water and ethyl alcohol; (iv) the obtained multilayer film was thermally treated in an oven, in a vacuum, at a temperature of 200°C, in order to decompose the intermediate organic compounds of Al, Si and P, with the formation of the mixed network AI2O3-S1O2-P2O5: (v) optical characterization of the obtained film, regarding transmission in the UV-Vis-NIR range and photoluminescence in the NIR range.
în Fig.l se prezintă aparatul utilizat pentru depunerea filmelor PbSl și PbS2 pe substrate de sticlă și respectiv, ITO, substratele avand dimensiunea de 2,5 x 2,5 mm2, decapate chimic înainte de utilizare. Aparatul este denumit “Spin coater WS-650SZ, Laurel Spinner, Laurell Technologies Corporation, North Wales, PA, USA.Fig.l shows the apparatus used for the deposition of PbSl and PbS2 films on glass and ITO substrates respectively, the substrates having the size of 2.5 x 2.5 mm 2 , chemically pickled before use. The device is called "Spin coater WS-650SZ, Laurel Spinner, Laurell Technologies Corporation, North Wales, PA, USA.
Reacțiile chimice care au loc în procesul de gelifiere, incluzând hidroliza și condensarea (eliminarea apei și a alcoolului etilic) sunt următoarele:The chemical reactions that take place in the gelation process, including hydrolysis and condensation (removal of water and ethyl alcohol) are as follows:
(CH3-CHO-CH3)3 Al + H-OH = (CH3-CHO-CH3)2A1-OH + CH3-CHOH-CH3(1) (CH3-CHO-CH3)2A1-OH + H-OH = CH3-CHO-CH3-A1-(OH)2 + CH3-CHOH-CH3 (2) (C2H5-O)4Si + H-OH = (C2H5-O)3Si-OH + C2H5-OH(3) (C2H5-O)3PO + HOH = (C2H5-O)2PO-OH + C2H5-OH(4)(CH 3 -CHO-CH 3 ) 3 Al + H-OH = (CH 3 -CHO-CH 3 ) 2 A1-OH + CH 3 -CHOH-CH 3 (1) (CH 3 -CHO-CH 3 ) 2 A1-OH + H-OH = CH 3 -CHO-CH 3 -A1-(OH) 2 + CH 3 -CHOH-CH 3 (2) (C 2 H 5 -O)4Si + H-OH = (C 2 H 5 -O) 3 Si-OH + C2H5-OH(3) (C 2 H 5 -O) 3 PO + HOH = (C 2 H 5 -O) 2 PO-OH + C2H5-OH(4)
CH3-CHO-CH3-A1-(OH)2 + (C2H5-O)3Si-OH = CH3-CHO-CH3-Al-OH-O-Si(C2H5-O)3 + H-OH(5)CH 3 -CHO-CH 3 -A1-(OH) 2 + (C 2 H 5 -O) 3 Si-OH = CH 3 -CHO-CH 3 -Al-OH-O-Si(C 2 H5-O) 3 + H-OH(5)
CH3-CHO-CH3-Al-OH-O-Si(C2H5-O)3 + (C2H5-O)2PO-OH = CH3-CHO-CH3-A1-(OPO-(C2H5-O)2)-(O-Si(C2H5-O)3) + H-OH(6)CH 3 -CHO-CH 3 -Al-OH-O-Si(C 2 H 5 -O) 3 + (C 2 H 5 -O)2PO-OH = CH 3 -CHO-CH 3 -A1-(OPO- (C 2 H5-O)2)-(O-Si(C 2 H5-O) 3 ) + H-OH(6)
CH3-CHO-CH3-Al-(O-PO-(C2H5-O)2)-(O-Si(C2H5-O)3) + 5H-OH = CH3-CHO-CH3Al-(O-PO-(OH)2)-O-Si-(OH)3 + 5C2H5-OH(7)CH 3 -CHO-CH 3 -Al-(O-PO-(C2H5-O)2)-(O-Si(C 2 H 5 -O) 3 ) + 5H-OH = CH 3 -CHO-CH 3 Al -(O-PO-(OH) 2 )-O-Si-(OH) 3 + 5C2H5-OH(7)
2CH3-CHO-CH3-Al-(O-PO-(OH)2)-O-Si-(OH)3 + O2 = 2CH3-CO-CH3 + A12O3 + P2O5 + 2SiO2 +6H2O(8)2CH 3 -CHO-CH 3 -Al-(O-PO-(OH) 2 )-O-Si-(OH) 3 + O 2 = 2CH 3 -CO-CH 3 + A1 2 O 3 + P2O5 + 2SiO 2 +6H2O(8)
Filmul obținut (PbSl) este relativ uniform și omogen, având culoare brună, specifică dopantului PbS.The obtained film (PbSl) is relatively uniform and homogeneous, having a brown color, specific to the PbS dopant.
Exemplul 2Example 2
Compoziția gravimetrică nominală a filmului dopat cu PbS (20 de depuneri succesive) pe substrat ITO, este: 2,97 % A12O3,13,39 % SiO2, 25,21 % P2O5, 58,41 % PbS (Cod PbS2).The nominal gravimetric composition of the PbS doped film (20 successive depositions) on the ITO substrate is: 2.97% A1 2 O 3 , 13.39% SiO 2 , 25.21% P 2 O 5 , 58.41% PbS (Code PbS2).
Volumele/cantitățile de reactanți utilizați pentru prepararea amestecului precursor, depus pe substrat rotativ de ITO, sunt identice cu cele prezentate în Tabelul 1.The volumes/amounts of reactants used to prepare the precursor mixture, deposited on the ITO spin substrate, are identical to those shown in Table 1.
Etapele metodei sol-gel, de sinteză a filmului dopat cu PbS, depus pe substrat de ITO (PbS2), sunt identice cu cele prezentate în exemplul 1 (PbSl). Capacitatea de umectate a soluției precursoare pe substratul ITO este diferită de cea a soluției precursoare pe substratul de sticlă. în consecință, viteza de rotație a substratului ITO a fostThe steps of the sol-gel method, for the synthesis of the film doped with PbS, deposited on an ITO substrate (PbS2), are identical to those presented in example 1 (PbSl). The wetting capacity of the precursor solution on the ITO substrate is different from that of the precursor solution on the glass substrate. consequently, the rotation speed of the ITO substrate was
2500-3000 rpm, urmărindu-se realizarea unei distribuții uniforme a soluției precursoare pe acest substrat.2500-3000 rpm, aiming to achieve a uniform distribution of the precursor solution on this substrate.
Reacțiile chimice care au loc în procesul de gelifiere, incluzând hidroliza și condensarea (eliminarea apei și a alcoolului etilic) sunt identice cu cele prezentate în exemplul 1.The chemical reactions that take place in the gelation process, including hydrolysis and condensation (removal of water and ethyl alcohol) are identical to those shown in example 1.
Filmul obținut este relativ uniform și omogen, având culoare brună, specifică dopantului PbS.The obtained film is relatively uniform and homogeneous, having a brown color, specific to the PbS dopant.
Transmisia optica a filmelor oxidice dopate cu PbS, depuse pe substrat de sticlă (PbSl), respectiv, ITO(PbS2), în domeniul UV-Vis-NIR, este prezentată în Tabelul 2.The optical transmission of oxide films doped with PbS, deposited on glass substrate (PbSl), respectively, ITO(PbS2), in the UV-Vis-NIR range, is presented in Table 2.
Tabelul 2. Transmisia optica a filmelor oxidice dopate cu PbS, depuse pe substrat de sticlă (PbSl), respectiv, ITO (PbS2).Table 2. Optical transmission of oxide films doped with PbS, deposited on glass substrate (PbSl), respectively, ITO (PbS2).
Limita de transmisie a filmului PbS 1 este 590 nm iar a filmului PbS2 este 794 nm.The transmission limit of the PbS 1 film is 590 nm and that of the PbS2 film is 794 nm.
în Tabelul 3 se prezintă caracteristicile fotoluminescenței în domeniul NIR a filmelor oxidice dopate cu PbS, depuse pe substrat de sticlă (PbSl), respectiv, ITO (PbS2), prin excitare la 800 nm.Table 3 shows the photoluminescence characteristics in the NIR range of PbS-doped oxide films, deposited on glass (PbSl) and ITO (PbS2) substrates, respectively, by excitation at 800 nm.
Tabelul 3. Caracteristicile fotoluminescenței în domeniul NIR, ale filmelor oxidice dopate cu PbS, depuse pe substrat de sticlă (PbSl), respectiv, ITO (PbS2), prin excitare la 800 nm.Table 3. Photoluminescence characteristics in the NIR range of oxide films doped with PbS, deposited on glass (PbSl) and ITO (PbS2) substrates respectively, by excitation at 800 nm.
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