MD4344C1 - Process for producing a luminiferous composite based on amorphous chalcogenide semiconductor As2S3 and coordinative compound Eu(TTA)2(Ph3PO)2NO3 - Google Patents
Process for producing a luminiferous composite based on amorphous chalcogenide semiconductor As2S3 and coordinative compound Eu(TTA)2(Ph3PO)2NO3 Download PDFInfo
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- MD4344C1 MD4344C1 MDA20140049A MD20140049A MD4344C1 MD 4344 C1 MD4344 C1 MD 4344C1 MD A20140049 A MDA20140049 A MD A20140049A MD 20140049 A MD20140049 A MD 20140049A MD 4344 C1 MD4344 C1 MD 4344C1
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- as2s3
- tta
- ph3po
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- 229910052958 orpiment Inorganic materials 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 150000001875 compounds Chemical class 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000004065 semiconductor Substances 0.000 title claims abstract description 16
- 150000004770 chalcogenides Chemical class 0.000 title abstract 2
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 4
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000004090 dissolution Methods 0.000 claims abstract description 3
- 238000000265 homogenisation Methods 0.000 claims abstract description 3
- 238000000151 deposition Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 2
- 230000003287 optical effect Effects 0.000 abstract description 10
- LNBHUCHAFZUEGJ-UHFFFAOYSA-N europium(3+) Chemical compound [Eu+3] LNBHUCHAFZUEGJ-UHFFFAOYSA-N 0.000 abstract description 5
- 230000005540 biological transmission Effects 0.000 abstract description 3
- 230000003321 amplification Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000003199 nucleic acid amplification method Methods 0.000 abstract description 2
- 239000013307 optical fiber Substances 0.000 abstract description 2
- 230000005693 optoelectronics Effects 0.000 abstract description 2
- 239000010409 thin film Substances 0.000 abstract 1
- 239000011521 glass Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 238000005424 photoluminescence Methods 0.000 description 9
- -1 polyethylene terephthalate Polymers 0.000 description 6
- 229920000139 polyethylene terephthalate Polymers 0.000 description 6
- 239000005020 polyethylene terephthalate Substances 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052798 chalcogen Inorganic materials 0.000 description 2
- 150000001787 chalcogens Chemical class 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910001940 europium oxide Inorganic materials 0.000 description 2
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 238000000103 photoluminescence spectrum Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000007669 thermal treatment Methods 0.000 description 2
- 238000000411 transmission spectrum Methods 0.000 description 2
- FIQMHBFVRAXMOP-UHFFFAOYSA-N triphenylphosphane oxide Chemical compound C=1C=CC=CC=1P(C=1C=CC=CC=1)(=O)C1=CC=CC=C1 FIQMHBFVRAXMOP-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 206010034972 Photosensitivity reaction Diseases 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 150000002178 europium compounds Chemical class 0.000 description 1
- GAGGCOKRLXYWIV-UHFFFAOYSA-N europium(3+);trinitrate Chemical compound [Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GAGGCOKRLXYWIV-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 230000005499 meniscus Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 230000036211 photosensitivity Effects 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- TXBBUSUXYMIVOS-UHFFFAOYSA-N thenoyltrifluoroacetone Chemical compound FC(F)(F)C(=O)CC(=O)C1=CC=CS1 TXBBUSUXYMIVOS-UHFFFAOYSA-N 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
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Abstract
Description
Invenţia se referă la un procedeu de obţinere a unui compozit luminofor pe baza semiconductorului calcogenic amorf As2S3 şi compusului coordinativ al europiului(III), sub formă de straturi subţiri şi fibre optice, care poate fi utilizat în industria optoelectronică, şi anume pentru producerea dispozitivelor fotoluminescente, pentru înregistrarea, transmiterea şi amplificarea informaţiei optice. The invention refers to a process for obtaining a luminophore composite based on the amorphous chalcogenous semiconductor As2S3 and the coordination compound of europium(III), in the form of thin layers and optical fibers, which can be used in the optoelectronic industry, namely for the production of photoluminescent devices , for recording, transmission and amplification of optical information.
Este cunoscut procedeul de obţinere a compozitului luminofor pe baza materialului semiconductor amorf As2S3 şi compusului europiului Eu2O3. The process of obtaining the luminophore composite based on the amorphous semiconductor material As2S3 and the europium compound Eu2O3 is known.
Matricele din compozite au fost obţinute prin metoda evaporării termice în vacuum pe substraturi de sticlă cu dimensiunile de 25x25 mm2 a ţintei aparte de As2S3 şi Eu2O3. În final după tratarea termică a stratului mixt în atmosferă de azot la 180°C timp de 90 min se obţine un compozit luminofor. În urma acestei tratări oxidul de europiu difuzează în stratul de As2S3 [1]. The composite matrices were obtained by the method of thermal evaporation in vacuum on glass substrates with the dimensions of 25x25 mm2 of the target apart from As2S3 and Eu2O3. Finally, after thermal treatment of the mixed layer in a nitrogen atmosphere at 180°C for 90 min, a luminophore composite is obtained. Following this treatment, europium oxide diffuses into the As2S3 layer [1].
Dezavantajele acestui procedeu de obţinere a compozitului constau în: The disadvantages of this process for obtaining the composite consist of:
- aplicarea aparatelor de vid, care sunt costisitoare; - application of vacuum devices, which are expensive;
- aplicarea procedeelor termice cu utilizarea temperaturilor înalte; - the application of thermal processes with the use of high temperatures;
- straturile subţiri din acest compozit, din cauza cristalizării parţiale a matricei amorfe As2S3 la tratarea termică cu temperaturi mari, sunt slab transparente şi nu pot fi utilizate în optică şi în fotonică; - the thin layers of this composite, due to the partial crystallization of the amorphous As2S3 matrix during heat treatment at high temperatures, are poorly transparent and cannot be used in optics and photonics;
- imposibilitatea de a depune straturi subtiri de compozit pe arii mari. - the impossibility of depositing thin layers of composite on large areas.
În calitate de cea mai apropiată soluţie serveşte procedeul de obţinere a compozitului luminofor pe baza materialului semiconductor amorf As2S3 şi compusului europiului(III) Eu2O3. Matricele din compozit au fost obţinute prin metoda depunerii laser pulsate pe substraturi de sticlă cu dimensiunile de 25x25 mm2 a ţintei aparte de As2S3 şi Eu2O3. În final după tratarea termică a stratului mixt în atmosferă de azot la 180°C timp de 45 min se obţine un compozit luminofor. În urma acestei tratări oxidul de europiu difuzează în stratul de As2S3 [2]. As the closest solution serves the process of obtaining the luminophore composite based on the amorphous semiconductor material As2S3 and the europium(III) Eu2O3 compound. The composite matrices were obtained by the method of pulsed laser deposition on glass substrates with dimensions of 25x25 mm2 of the target apart from As2S3 and Eu2O3. Finally, after thermal treatment of the mixed layer in a nitrogen atmosphere at 180°C for 45 min, a luminophore composite is obtained. Following this treatment, europium oxide diffuses into the As2S3 layer [2].
Dezavantajele acestui procedeu de obţinere a compozitului constau în: The disadvantages of this process for obtaining the composite consist of:
- aplicarea instalaţiei laser, care este costisitoare; - application of the laser installation, which is expensive;
- aplicarea procedeelor termice cu utilizarea temperaturilor înalte; - the application of thermal processes with the use of high temperatures;
- straturile subţiri din acest compozit, din cauza cristalizării parţiale a matricei amorfe As2S3 la tratarea termică cu temperaturi mari, sunt slab transparente şi nu pot fi utilizate în optică şi în fotonică, - the thin layers of this composite, due to the partial crystallization of the amorphous As2S3 matrix during heat treatment at high temperatures, are poorly transparent and cannot be used in optics and photonics,
- imposibilitatea de a depune straturi subtiri de compozit pe arii mari. - the impossibility of depositing thin layers of composite on large areas.
Problema pe care o rezolvă invenţia constă în elaborarea unui procedeu de obţinere a compozitului fotosensibil şi luminofor dintr-un semiconductor calcogenic amorf (de exemplu, As2S3) şi compusul coordinativ al europiului(III), în care se menţine structura moleculară şi proprietăţile optice ale fiecărei componente aparte în compozit: a semiconductorului calcogenic amorf şi compusului coordinativ Eu(TTA)2(Ph3PO)2NO3. The problem that the invention solves consists in the development of a process for obtaining the photosensitive and luminophore composite from an amorphous chalcogenic semiconductor (for example, As2S3) and the coordinating compound of europium(III), in which the molecular structure and optical properties of each are maintained separate components in the composite: of the amorphous chalcogenic semiconductor and the coordination compound Eu(TTA)2(Ph3PO)2NO3.
Problema se rezolvă prin aceea că procedeul de obţinere a unui compozit luminofor pe baza semiconductorului calcogenic amorf As2S3 şi compusului coordinativ Eu(TTA)2(Ph3PO)2NO3 include dizolvarea separată a semiconductorului As2S3 şi compusului Eu(TTA)2(Ph3PO)2NO3 în propilamină sau monoetanolamină la temperatura de 18…25°C, timp de 4…20 ore, amestecarea acestor soluţii pentru obţinerea compozitului cu următorul raport masic, %: Eu(TTA)2(Ph3PO)2NO3 - 2,0…20,0, As2S3 - restul, şi omogenizarea la temperatura de 18…25°C şi o presiune atmosferică normală, timp de 20…30 ore, depunerea amestecului lichid obţinut pe un substrat şi uscarea la temperatura de 45…50°C timp de 3…5 ore. The problem is solved by the fact that the process for obtaining a luminophore composite based on the amorphous chalcogenous semiconductor As2S3 and the coordinating compound Eu(TTA)2(Ph3PO)2NO3 includes the separate dissolution of the semiconductor As2S3 and the compound Eu(TTA)2(Ph3PO)2NO3 in propylamine or monoethanolamine at a temperature of 18...25°C, for 4...20 hours, mixing these solutions to obtain the composite with the following mass ratio, %: Eu(TTA)2(Ph3PO)2NO3 - 2.0...20.0, As2S3 - the rest, and homogenization at a temperature of 18...25°C and a normal atmospheric pressure, for 20...30 hours, depositing the obtained liquid mixture on a substrate and drying at a temperature of 45...50°C for 3...5 hours.
Rezultatul tehnic al invenţiei constă în următoarele: The technical result of the invention consists of the following:
- posibilitatea simplă de a obţine un material cu fotosensibilitate şi luminozitate optimă pentru înscrierea informaţiei holografice; - the simple possibility of obtaining a material with optimal photosensitivity and brightness for recording holographic information;
- pentru obţinerea compusului nu este necesară aplicarea tehnicii de vid, a laserului, a temperaturilor înalte; - to obtain the compound, it is not necessary to apply the vacuum technique, the laser, or high temperatures;
- asigurarea gradului înalt de omogenitate al compozitelor, - ensuring the high degree of homogeneity of the composites,
- posibilitatea de dirijare a tehnologiei, proprietăţilor optice şi altor parametri ai compozitului prin variaţia componenţei mixte. - the possibility of directing the technology, optical properties and other parameters of the composite by varying the mixed composition.
Rezultatul dat se obţine datorită gradului înalt de omogenitate al materialelor fotosensibile confecţionate din soluţii chimice de semiconductori calcogenici amorfi, în care se obţine doparea optimă a materialului cu ioni Eu3+. Materialul este obţinut în condiţii normale de presiune şi temperatură pe diferite suporturi. The given result is obtained due to the high degree of homogeneity of the photosensitive materials made from chemical solutions of amorphous chalcogenous semiconductors, in which the optimal doping of the material with Eu3+ ions is obtained. The material is obtained under normal conditions of pressure and temperature on different supports.
Invenţia se explică cu ajutorul desenelor din fig. 1-5, care reprezintă: The invention is explained with the help of the drawings in fig. 1-5, which represent:
- fig. 1, formula de structură a compusului coordinativ Eu(TTA)2(Ph3PO)2NO3, - fig. 1, the structural formula of the coordination compound Eu(TTA)2(Ph3PO)2NO3,
- fig. 2, schema mostrei cu compozit fotoluminofor pe substrat, unde 3 este un suport din polietilentereftalat sau sticlă, 2 - strat subţire de metal (cu rezistivitatea superficială de 105 Om/cm2, grosimea de ~ 100 Å), 1 - strat din compozit fotoluminofor; - fig. 2, scheme of the sample with photoluminescent composite on the substrate, where 3 is a support made of polyethylene terephthalate or glass, 2 - thin metal layer (with surface resistivity of 105 Ohm/cm2, thickness of ~ 100 Å), 1 - layer of photoluminescent composite;
- fig. 3, spectrul de transmisie al compozitului As2S3/Eu(TTA)2(Ph3PO)2NO3 pentru concentraţia de 10% de Eu(TTA)2(Ph3PO)2NO3 în compozit, - fig. 3, the transmission spectrum of the As2S3/Eu(TTA)2(Ph3PO)2NO3 composite for the 10% concentration of Eu(TTA)2(Ph3PO)2NO3 in the composite,
- fig. 4, spectrul de transparenţă al stratului Eu(TTA)2(Ph3PO)2NO3, - fig. 4, the transparency spectrum of the Eu(TTA)2(Ph3PO)2NO3 layer,
- fig. 5, spectrul de fotoluminescenţă al stratului subţire de compozit As2S3/Eu(TTA)2(Ph3PO)2NO3 pentru concentraţia de 10% de Eu(TTA)2(Ph3PO)2NO3 în compozit. - fig. 5, the photoluminescence spectrum of the As2S3/Eu(TTA)2(Ph3PO)2NO3 composite thin layer for the 10% concentration of Eu(TTA)2(Ph3PO)2NO3 in the composite.
Exemple de realizare a invenţiei Examples of realization of the invention
Exemplul 1 Example 1
În condiţii normale de temperatură şi presiune se pregăteşte soluţia care conţine As2S3 şi propilamină în următorul raport: As2S3 - 8 mg, propilamină - 2 ml. Soluţia se pregăteşte la temperatura de 18...25°C timp de 4...20 ore, la agitare continuă. Amestecul final reprezintă un lichid omogen de culoare galbenă deschisă. Din amestecul obţinut se prepară probele necesare pe diferite substraturi (sticlă, polietilentereftalat etc.), sub formă de straturi, care se usucă în termostat la temperatura de 45...50°C timp de 3...5 ore. Under normal conditions of temperature and pressure, prepare the solution containing As2S3 and propylamine in the following ratio: As2S3 - 8 mg, propylamine - 2 ml. The solution is prepared at a temperature of 18...25°C for 4...20 hours, with continuous stirring. The final mixture is a light yellow homogeneous liquid. From the mixture obtained, the necessary samples are prepared on different substrates (glass, polyethylene terephthalate, etc.), in the form of layers, which are dried in a thermostat at a temperature of 45...50°C for 3...5 hours.
Exemplul 2 Example 2
În condiţii normale de temperatură şi presiune se pregătesc două tipuri de soluţii. Soluţia 1 conţine As2S3 şi propilamină în următorul raport: As2S3 - 8 mg, propilamină - 2 ml. Soluţia 2 conţine compusul coordinativ Eu(TTA)2(Ph3PO)2NO3 - 2 mg şi propilamină - 1 ml. Soluţiile 1 şi 2 se pregătesc la temperatura de 18...25°C timp de 4...20 ore, la agitare continuă. Apoi soluţiile 1 şi 2 se amestecă şi se agită continuu la temperatura de 18...25°C timp de 20...30 ore. Amestecul final reprezintă un lichid omogen de culoare galbenă deschisă. Din amestecul obţinut se prepară probele necesare pe diferite substraturi (sticlă, polietilentereftalat etc.), sub formă de straturi, care se usucă în termostat la temperatura de 45...50°C timp de 3...5 ore. Under normal conditions of temperature and pressure, two types of solutions are prepared. Solution 1 contains As2S3 and propylamine in the following ratio: As2S3 - 8 mg, propylamine - 2 ml. Solution 2 contains the coordinating compound Eu(TTA)2(Ph3PO)2NO3 - 2 mg and propylamine - 1 ml. Solutions 1 and 2 are prepared at a temperature of 18...25°C for 4...20 hours, with continuous stirring. Then solutions 1 and 2 are mixed and stirred continuously at a temperature of 18...25°C for 20...30 hours. The final mixture is a light yellow homogeneous liquid. From the mixture obtained, the necessary samples are prepared on different substrates (glass, polyethylene terephthalate, etc.), in the form of layers, which are dried in a thermostat at a temperature of 45...50°C for 3...5 hours.
Exemplul 3 Example 3
În condiţii normale de temperatură şi presiune se pregătesc două tipuri de soluţii. Soluţia 1 conţine As2S3 şi propilamină în următorul raport: As2S3 - 18 mg, propilamină - 2 ml. Soluţia 2 conţine compusul coordinativ Eu(TTA)2(Ph3PO)2NO3 - 2 mg şi propilamină - 1 ml. Soluţiile 1 şi 2 se pregătesc la temperatura de 18...25°C timp de 4...20 ore, la agitare continuă. Apoi soluţiile 1 şi 2 se amestecă şi se agită continuu la temperatura de 18...25°C timp de 20...30 ore. Amestecul final reprezintă un lichid omogen de culoare galbenă deschisă. Din amestecul obţinut se prepară probele necesare pe diferite substraturi (sticlă, polietilentereftalat etc.), sub formă de straturi, care se usucă în termostat la temperatura de 45...50°C timp de 3...5 ore. Under normal conditions of temperature and pressure, two types of solutions are prepared. Solution 1 contains As2S3 and propylamine in the following ratio: As2S3 - 18 mg, propylamine - 2 ml. Solution 2 contains the coordinating compound Eu(TTA)2(Ph3PO)2NO3 - 2 mg and propylamine - 1 ml. Solutions 1 and 2 are prepared at a temperature of 18...25°C for 4...20 hours, with continuous stirring. Then solutions 1 and 2 are mixed and stirred continuously at a temperature of 18...25°C for 20...30 hours. The final mixture is a light yellow homogeneous liquid. From the mixture obtained, the necessary samples are prepared on different substrates (glass, polyethylene terephthalate, etc.), in the form of layers, which are dried in a thermostat at a temperature of 45...50°C for 3...5 hours.
Exemplul 4 Example 4
În condiţii normale de temperatură şi presiune se pregătesc două tipuri de soluţii. Soluţia 1 conţine As2S3 şi propilamină în următorul raport: As2S3 - 49 mg, propilamină - 4 ml. Soluţia 2 conţine compusul coordinativ Eu(TTA)2(Ph3PO)2NO3 - 1 mg şi propilamină - 1 ml. Soluţiile 1 şi 2 se pregătesc la temperatura de 18...25°C timp de 4...20 ore, la agitare continuă. Apoi soluţiile 1 şi 2 se amestecă şi se agită continuu la temperatura de 18...25°C timp de 20...30 ore. Amestecul final reprezintă un lichid omogen de culoare galbenă deschisă. Din amestecul obţinut se prepară probele necesare pe diferite substraturi (sticlă, polietilentereftalat etc.), sub formă de straturi, care se usucă în termostat la temperatura de 45...50°C timp de 3...5 ore. Under normal conditions of temperature and pressure, two types of solutions are prepared. Solution 1 contains As2S3 and propylamine in the following ratio: As2S3 - 49 mg, propylamine - 4 ml. Solution 2 contains the coordinating compound Eu(TTA)2(Ph3PO)2NO3 - 1 mg and propylamine - 1 ml. Solutions 1 and 2 are prepared at a temperature of 18...25°C for 4...20 hours, with continuous stirring. Then solutions 1 and 2 are mixed and stirred continuously at a temperature of 18...25°C for 20...30 hours. The final mixture is a light yellow homogeneous liquid. From the mixture obtained, the necessary samples are prepared on different substrates (glass, polyethylene terephthalate, etc.), in the form of layers, which are dried in a thermostat at a temperature of 45...50°C for 3...5 hours.
Exemplul 5 Example 5
În condiţii normale de temperatură şi presiune se pregăteşte soluţia care conţine compusul coordinativ Eu(TTA)2(Ph3PO)2NO3 - 1 mg şi propilamină - 1 ml. Soluţia se pregăteşte la temperatura de 18...25°C timp de 4...20 ore. Soluţia finală reprezintă un lichid omogen fără culoare. Din soluţia obţinută se prepară probele necesare pe diferite substraturi (sticlă, polietilentereftalat etc.), sub formă de straturi, care se usucă în termostat la temperatura de 45...50°C timp de 3...5 ore. Under normal conditions of temperature and pressure, prepare the solution containing the coordinating compound Eu(TTA)2(Ph3PO)2NO3 - 1 mg and propylamine - 1 ml. The solution is prepared at a temperature of 18...25°C for 4...20 hours. The final solution is a colorless homogeneous liquid. From the solution obtained, the necessary samples are prepared on different substrates (glass, polyethylene terephthalate, etc.), in the form of layers, which are dried in a thermostat at a temperature of 45...50°C for 3...5 hours.
Compusul coordinativ Eu(TTA)2(Ph3PO)2NO3 bis(tenoiltrifluoroacetonato)bis(trifenil-fosfinoxid)(mononitrat)europiu(III) a fost obţinut după metoda analogică descrisă în literatură (Verlan V., Iovu M., Culeac I., Nistor Y., Turta C., Zubareva V. Photoluminescence properties of PVP/Eu(TTA)2(Phen3PO)2NO3 nanocomposites. Journal of Non-Crystalline Solids, 2011, 357, p. 1004-1007). The coordinating compound Eu(TTA)2(Ph3PO)2NO3 bis(thenoyltrifluoroacetonato)bis(triphenyl-phosphine oxide)(mononitrate) europium(III) was obtained according to the analogous method described in the literature (Verlan V., Iovu M., Culeac I., Nistor Y., Turta C., Zubareva V. Photoluminescence properties of PVP/Eu(TTA)2(Phen3PO)2NO3 nanocomposites. Journal of Non-Crystalline Solids, 2011, 357, p. 1004-1007).
Sinteza compusului coordinativ Eu(TTA)2(Ph3PO)2NO3 Synthesis of the coordination compound Eu(TTA)2(Ph3PO)2NO3
În 10 ml de etanol (96%) fierbinte (40...60°C) au fost dizolvate 0,44 g (2 mmol) de tenoiltrifluoroacetonă şi 0,56 g (2 mmol) de trifenilfosfinoxid. La soluţia obţinută s-au adăugat 2 ml soluţie de hidroxid de sodiu. Apoi a fost adăugată prin picurare la amestecare continuă soluţia din 1 mmol de nitrat de europiu în 5 ml de арă. În amestec s-a format imediat un precipitat în formă de cremă de culoare brună-deschisă. Precipitatul a fost filtrat, spălat cu etanol, uscat complet în aer. S-a obţinut compusul coordinativ cu masa de 0,85 g, randamentul sintezei este de 69,9%. 0.44 g (2 mmol) of thenoyltrifluoroacetone and 0.56 g (2 mmol) of triphenylphosphine oxide were dissolved in 10 ml of ethanol (96%) hot (40...60°C). 2 ml of sodium hydroxide solution were added to the obtained solution. Then the solution of 1 mmol of europium nitrate in 5 ml of ara was added dropwise with continuous mixing. A light brown cream precipitate immediately formed in the mixture. The precipitate was filtered, washed with ethanol, dried completely in air. The coordinating compound with a mass of 0.85 g was obtained, the yield of the synthesis is 69.9%.
Pentru C52H38F6EuNO9P2S2 For C52H38F6EuNO9P2S2
Calculat, %: С = 51,49; H = 3,16; N = 1,15; S = 5,28. Calculated, %: С = 51.49; H = 3.16; N = 1.15; S = 5.28.
Determinat, %: С = 51,49; H = 3,48; N = 0,95; S = 5,14. Determined, %: С = 51.49; H = 3.48; N = 0.95; S = 5.14.
Depunerea compozitului fotoluminofor se efectuează prin metode cunoscute în literatură: metoda de depunere prin picături, metoda de „menisc”, metoda de centrifugare cu ajutorul unor dispozitive mecanice etc. Grosimea stratului de compozit fotoluminofor este dirijabilă şi variază în funcţie de concentraţia semiconductorului în soluţie, de tehnologia de depunere etc. Grosimea straturilor fotosensibile constituie de obicei 0,2...6,0 µm. Proprietăţile optice şi fotoluminescenţa straturilor fotoluminofore au fost cercetate prin metode spectrale. Pentru măsurările optice de transmisie în domeniile de lungimi de undă ultraviolet - vizibil (200...800 nm) s-au utilizat aparatele Specord-UV şi VIS, firma CARL ZEISS Jena, iar pentru măsurarea fotoluminescenţei - monocromatorul MDR-12 dirijate de computer. Măsurările s-au efectuat la temperatura de 18...25ºC la excitarea fotoluminescenţei cu radiaţie laser N2 (λ = 0,337 µm). Calculul parametrilor optici şi al pragului lor de absorbţie a fost efectuat cu ajutorul metodei descrise în literatură (Swanepoel R. Determination of the thickness and optical constants of amorphous silicon. Journal of Physics E: Scientific Instruments, 1983, vol. 16, p. 1214-1222). The deposition of the photoluminescent composite is carried out by methods known in the literature: the droplet deposition method, the "meniscus" method, the centrifugation method with the help of mechanical devices, etc. The thickness of the photoluminescent composite layer is adjustable and varies depending on the concentration of the semiconductor in the solution, the deposition technology, etc. The thickness of photosensitive layers is usually 0.2...6.0 µm. The optical properties and photoluminescence of the photoluminescent layers were investigated by spectral methods. Specord-UV and VIS devices, manufactured by CARL ZEISS Jena, were used for optical transmission measurements in the ultraviolet-visible wavelength range (200...800 nm), and for photoluminescence measurements - the computer-controlled MDR-12 monochromator . The measurements were performed at a temperature of 18...25ºC upon photoluminescence excitation with N2 laser radiation (λ = 0.337 µm). The calculation of the optical parameters and their absorption threshold was carried out using the method described in the literature (Swanepoel R. Determination of the thickness and optical constants of amorphous silicon. Journal of Physics E: Scientific Instruments, 1983, vol. 16, p. 1214 -1222).
Măsurările spectrelor de transmisie ale straturilor subţiri ale compozitului As2S3/Eu(TTA)2(Ph3PO)2NO3 au arătat coincidenţa pragului lor de absorbţie cu cel al stratului din materialul chalcogenic As2S3, ceea ce demonstrează că structura moleculară a compozitului se menţine aceeaşi şi serveşte ca matrice pentru nanocristalele de Eu(TTA)2(Ph3PO)2NO3. În afară de aceasta, pragul corespunde pragului de absorbţie cunoscut din literatură pentru semiconductorul calcogenic amorf As2S3 respectiv (Swanepoel R. Determination of the thickness and optical constants of amorphous silicon. Journal of Physics E: Scientific Instruments, 1983, vol. 16, p. 1214-1222 şi Popescu M., Andrieş A., Ciumaş V., Iovu M., Şutov S., Ţiuleanu D. Fizica sticlelor calcogenice, „I.E.P. Ştiinţa”, 1996, Chişinău, p. 486), obţinut prin metoda de evaporare termică în vid din material sintetizat As2S3. În spectrul de fotoluminescenţă al compozitului As2S3/Eu(TTA)2(Ph3PO)2NO3 se evidenţiază maximumurile de luminescenţă caracteristice ionului Eu3+ 5D0 ###U2247Fi (i = (0,1,2,3,4,5) (fig. 4), banda principală de emisie 5D0 ###U2247F2 este centrată la 612 nm. The measurements of the transmission spectra of the thin layers of the As2S3/Eu(TTA)2(Ph3PO)2NO3 composite showed the coincidence of their absorption threshold with that of the As2S3 chalcogen material layer, which proves that the molecular structure of the composite remains the same and serves as matrix for Eu(TTA)2(Ph3PO)2NO3 nanocrystals. Apart from this, the threshold corresponds to the absorption threshold known from the literature for the respective amorphous chalcogen semiconductor As2S3 (Swanepoel R. Determination of the thickness and optical constants of amorphous silicon. Journal of Physics E: Scientific Instruments, 1983, vol. 16, p. 1214-1222 and Popescu M., Andries A., Ciumaş V., Iovu M., Şutov S., Ţiuleanu D. Physics of chalcogenous glasses, "I.E.P. Ştiinţa", 1996, Chişinău, p. 486), obtained by the evaporation method vacuum thermal from synthesized material As2S3. In the photoluminescence spectrum of the As2S3/Eu(TTA)2(Ph3PO)2NO3 composite, the luminescence maxima characteristic of the ion Eu3+ 5D0 ###U2247Fi (i = (0,1,2,3,4,5)) are highlighted (fig. 4 ), the main emission band of 5D0 ###U2247F2 is centered at 612 nm.
Dependenţa intensităţii fotoluminescenţei de concentraţia compusului coordinativ Eu(TTA)2(Ph3PO)2NO3 în compozitul As2S3/Eu(TTA)2(Ph3PO)2NO3 este arătată în tabel. Cu creşterea concentraţiei Eu(TTA)2(Ph3PO)2NO3 în As2S3 intensitatea de fotoluminescenţă creşte cu o tendinţă de saturare. Măsurarea fotoluminescenţei a tuturor probelor a fost efectuată în aceleaşi condiţii de excitare. The dependence of the photoluminescence intensity on the concentration of the coordinating compound Eu(TTA)2(Ph3PO)2NO3 in the As2S3/Eu(TTA)2(Ph3PO)2NO3 composite is shown in the table. With increasing Eu(TTA)2(Ph3PO)2NO3 concentration in As2S3, the photoluminescence intensity increases with a saturation tendency. Photoluminescence measurement of all samples was performed under the same excitation conditions.
După cum se observă în fig. 4 spectrul de transparenţă optică are pragul de absorbţie care corespunde pragului de absorbţie cunoscut din literatură pentru semiconductorul calcogenic amorf As2S3, obţinut prin metoda de evaporare în vid din material sintetizat separat. As seen in fig. 4 the optical transparency spectrum has the absorption threshold that corresponds to the absorption threshold known from the literature for the amorphous chalcogenous semiconductor As2S3, obtained by the vacuum evaporation method from separately synthesized material.
Tabel Table
Parametrii caracteristici ai straturilor subţiri din compozitul As2S3/ Eu(TTA)2(Ph3PO)2NO3 The characteristic parameters of the thin layers of the As2S3/ Eu(TTA)2(Ph3PO)2NO3 composite
Concentraţia Eu(TTA)2(Ph3PO)2- NO3 în compozit, % Banda energetică interzisă a com-pusului, eV Poziţia maximu-mului dominant de fotoluminescenţă, nm Intensitatea integrală de fotoluminescenţă, un. rel. 0 2.45 - - 2,00 2.45 612 250 10,00 2.48 614 800 20,00 2.52 613 1200 100,00 3.52 612 2500 The concentration of Eu(TTA)2(Ph3PO)2- NO3 in the composite, % The forbidden energy band of the compound, eV The position of the dominant photoluminescence maximum, nm The integral photoluminescence intensity, un. rel. 0 2.45 - - 2.00 2.45 612 250 10.00 2.48 614 800 20.00 2.52 613 1200 100.00 3.52 612 2500
1. Popescu M., Velea A., Simandan I. D., Sava F., Lőrinczi A., Ghervase L., Pavelescu G., Mihailescu I. N., Socol G., Georgescu S. Luminescence of arsenic sulphide dots doped with europium, prepared by thermal evaporation and pulsed laser deposition methods. Chalcogenide Letters, 2011, vol. 8, nr. 12, p. 719-724 1. Popescu M., Velea A., Simandan I. D., Sava F., Lőrinczi A., Ghervase L., Pavelescu G., Mihailescu I. N., Socol G., Georgescu S. Luminescence of arsenic sulphide dots doped with europium, prepared by thermal evaporation and pulsed laser deposition methods. Chalcogenide Letters, 2011, vol. 8, no. 12, pp. 719-724
2. Popescu M., Lőrinczi A., Velea A., Simandan I. D., Sava F., Pavelescu G., Niciu G. H., Niciu D. O., Mihailescu I. N., Socol G., Stefan N. Luminescence of europium in arsenic sulphide matrix. Chalcogenide Letters, 2011, vol. 8, nr. 11, p. 699-702 2. Popescu M., Lőrinczi A., Velea A., Simandan I. D., Sava F., Pavelescu G., Niciu G. H., Niciu D. O., Mihailescu I. N., Socol G., Stefan N. Luminescence of europium in arsenic sulphide matrix. Chalcogenide Letters, 2011, vol. 8, no. 11, pp. 699-702
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