MD1740Z - Method for producing epitaxial TiO2 thin layers - Google Patents

Method for producing epitaxial TiO2 thin layers Download PDF

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Publication number
MD1740Z
MD1740Z MDS20230010A MDS20230010A MD1740Z MD 1740 Z MD1740 Z MD 1740Z MD S20230010 A MDS20230010 A MD S20230010A MD S20230010 A MDS20230010 A MD S20230010A MD 1740 Z MD1740 Z MD 1740Z
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Moldova
Prior art keywords
tio2
vapors
flow
titanium isopropoxide
reactor
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MDS20230010A
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Romanian (ro)
Russian (ru)
Inventor
Василе БОТНАРЮК
Леонид ГОРЧАК
Симион РАЕВСКИЙ
Корнелиу РОТАРУ
Серджиу ВАТАВУ
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Публичное Учреждение Государственный Университет Молдовы
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Priority to MDS20230010A priority Critical patent/MD1740Z/en
Publication of MD1740Y publication Critical patent/MD1740Y/en
Publication of MD1740Z publication Critical patent/MD1740Z/en

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Abstract

The invention relates to the semiconductor manufacturing technology, and can be used for manufacturing optoelectronic devices.The method for producing epitaxial TiO2 thin layers comprises degreasing a glass substrate in toluene, drying it in isopropyl alcohol vapors and placing it in a chemical vapor deposition reactor, which is purged with argon for 20 min at a flow rate of 100 cm3/min, after which the temperature of the substrate is increased up to 400°C. The method also includes the formation of titanium isopropoxide vapors by bubbling at a temperature of 90°C. The deposition of epitaxial TiO2 layers is carried out by separately feeding into the reactor titanium isopropoxide vapors, carried by an argon flow at a speed of 40 cm3/min, and an oxygen flow at a speed of 40 cm3/min, for 30 min.

Description

Invenţia se referă la tehnologia de obţinere a semiconductoarelor, şi poate fi utilizată pentru fabricarea dispozitivelor optoelectronice. The invention refers to the technology of obtaining semiconductors, and can be used for the manufacture of optoelectronic devices.

Este cunoscut un procedeu de preparare a straturilor TiO2 prin metoda MOCVD (Metalorganic chemical vapour deposition) pentru diferite temperaturi a tetraizopropoxidului de titan. În acest caz straturile au fost crescute la temperaturi de 60°C, 65°C şi 75°C cu temperatura substratului de 400°C. Straturile au fost crescute pe substraturi de sticlă, preventiv spălate cu acetonă, etanol şi apă deionizată, la presiunea în reactor de 8,2·10-2 Torr, fără utilizarea barbotării tetraizopropoxidului de titan [1]. A process for preparing TiO2 layers by the MOCVD (Metalorganic chemical vapor deposition) method for different temperatures of titanium tetraisopropoxide is known. In this case the layers were grown at temperatures of 60°C, 65°C and 75°C with a substrate temperature of 400°C. The layers were grown on glass substrates, pre-washed with acetone, ethanol and deionized water, at the reactor pressure of 8.2·10-2 Torr, without the use of titanium tetraisopropoxide bubbling [1].

Neajunsul acestui procedeu constă în faptul ca straturile de TiO2 au o perfecţiune cristalină joasă. The shortcoming of this process lies in the fact that the TiO2 layers have a low crystalline perfection.

Cea mai apropiată soluţie tehnică de obţinere a straturilor de TiO2 prin metoda MOCVD este procedeul de depunere a straturilor de TiO2 la temperatura izopropoxidului de titan 90°C. Straturile subţiri de TiO2 au fost depuse pe substraturi de sticlă. Izopropoxidul de titan a fost menţinut în barbotor, încălzit până la 90°C şi transportat în reactor cu ajutorul oxigenului pur. Straturile au fost depuse la temperatura substraturilor de 400°C, la presiunea în reactor de 0,5 Torr pentru un debit a oxigenului de 7 cm3/min [2]. The closest technical solution for obtaining TiO2 layers by the MOCVD method is the process of depositing TiO2 layers at the temperature of titanium isopropoxide 90°C. Thin layers of TiO2 were deposited on glass substrates. The titanium isopropoxide was kept in the bubbler, heated to 90°C and transported into the reactor with the help of pure oxygen. The layers were deposited at a substrate temperature of 400°C, at a reactor pressure of 0.5 Torr for an oxygen flow rate of 7 cm3/min [2].

Neajunsul acestui procedeu constă în faptul ca nu este posibil de schimbat raportul dintre presiunea vaporilor izopropoxidului de titan şi fluxului de oxigen, ceea ce nu permite schimbarea raportului dintre fluxul de izopropoxid de titan şi fluxul de oxigen. The shortcoming of this process is that it is not possible to change the ratio between the titanium isopropoxide vapor pressure and the oxygen flow, which does not allow changing the ratio between the titanium isopropoxide flow and the oxygen flow.

Problema pe care o soluţionează prezenta invenţie constă în separarea vaporilor de izopropoxid de titan şi fluxului de oxigen, fapt care ar conduce la reglarea raportului dintre fluxul de izopropoxid de titan şi fluxul de oxigen, precum şi în majorarea rezistenţei stratului epitaxial. The problem that the present invention solves consists in the separation of the titanium isopropoxide vapors and the oxygen flow, a fact that would lead to the regulation of the ratio between the titanium isopropoxide flow and the oxygen flow, as well as in increasing the resistance of the epitaxial layer.

Procedeul de obţinere a straturilor epitaxiale subţiri de TiO2, conform invenţiei, înlătură dezavantajele menţionate mai sus prin aceea că include degresarea unui substrat de sticlă în toluen, uscarea lui în vapori de alcool izopropilic şi plasarea acestuia într-un reactor de depunere chimică din faza de vapori, care se purjează cu argon timp de 20 min cu viteza fluxului de 100 cm3/min, apoi se măreşte temperatura substratului până la 400°C. Procedeul de asemenea include producerea vaporilor de izopropoxid de titan prin barbotare la temperatura de 90°C. Depunerea straturilor epitaxiale de TiO2 se realizează prin debitarea separată în reactor a vaporilor de izopropoxid de titan, transportaţi cu un flux de argon cu viteza de 40 cm3/min, şi unui flux de oxigen cu viteza de 40 cm3/min, timp de 30 min. The process for obtaining thin epitaxial layers of TiO2, according to the invention, removes the disadvantages mentioned above in that it includes degreasing a glass substrate in toluene, drying it in isopropyl alcohol vapors and placing it in a chemical deposition reactor from the phase of vapors, which are purged with argon for 20 min at a flow rate of 100 cm3/min, then the substrate temperature is increased to 400°C. The process also includes the production of titanium isopropoxide vapor by bubbling at a temperature of 90°C. The deposition of the epitaxial TiO2 layers is carried out by separate discharge in the reactor of the titanium isopropoxide vapors, transported with an argon flow at a speed of 40 cm3/min, and an oxygen flow at a speed of 40 cm3/min, for 30 min .

Rezultatul tehnic al invenţiei constă în asigurarea posibilităţii reglării raportului dintre fluxul de izopropoxid de titan şi fluxul de oxigen, care îi conferă stratului epitaxial de TiO2 rezistenţă sporită. The technical result of the invention consists in ensuring the possibility of adjusting the ratio between the flow of titanium isopropoxide and the flow of oxygen, which gives the TiO2 epitaxial layer increased resistance.

Rezultatul tehnic obţinut se datorează faptului că fluxul de izopropoxid de titan şi fluxul de oxigen sunt introduse în reactor separat. The technical result obtained is due to the fact that the flow of titanium isopropoxide and the flow of oxygen are introduced into the reactor separately.

Exemplul de realizare a procedeului The example of making the procedure

Procedeul de obţinere a straturilor epitaxiale subţiri a TiO2 constă în degresarea substratului de sticlă în toluen, uscarea în vapori de alcool izopropilic şi plasarea acestuia în reactorul de depunere chimică din faza de vapori. Reactorul se purjează cu argon timp de 20 min cu viteza fluxului de 100 cm3/min, apoi se măreşte temperatura substratului până la 400°C. Într-un barbotor se produc vapori de izopropoxid de titan la temperatura de 90°C. Depunerea straturilor epitaxiale de TiO2 se realizează prin debitarea separată în reactor a vaporilor de izopropoxid de titan, transportaţi cu fluxul de argon, şi fluxului de oxigen. Fluxul de oxigen este debitat în reactor printr-un canal separat. Se efectuează depunerea stratului de TiO2 la un flux de 40 cm3/min de argon şi 40 cm3/min de oxigen. Durata de depunere este de 30 min. The procedure for obtaining thin epitaxial layers of TiO2 consists in degreasing the glass substrate in toluene, drying in isopropyl alcohol vapors and placing it in the chemical vapor deposition reactor. The reactor is purged with argon for 20 min at a flow rate of 100 cm3/min, then the temperature of the substrate is increased to 400°C. Titanium isopropoxide vapor is produced in a bubbler at 90°C. The deposition of the epitaxial TiO2 layers is achieved by the separate discharge in the reactor of the titanium isopropoxide vapors, transported with the argon flow, and the oxygen flow. The oxygen flow is discharged into the reactor through a separate channel. The TiO2 layer is deposited at a flow of 40 cm3/min of argon and 40 cm3/min of oxygen. The submission time is 30 min.

Procedeul descris îi conferă stratului epitaxial de TiO2 rezistenţă sporită. The described process gives the TiO2 epitaxial layer increased resistance.

1. Sang Hum Nam, Sang Jin Cho, Jin Hyo Boo. Growth behavior of titanium dioxide thin films at different precursor temperatures, Nanoscale Research Letters, 2012, nr. 7, art. nr. 89 1. Sang Hum Nam, Sang Jin Cho, Jin Hyo Boo. Growth behavior of titanium dioxide thin films at different precursor temperatures, Nanoscale Research Letters, 2012, no. 7, art. no. 89

2. M. I. B. Bernardi, E. J. H. Lee, P. N. Lisboa-Filho, E. R. Leite, E. Longo, J. A. Varela. TiO2 thin film growth using the MOCVD method, Materials Research, 2001, nr. 4(3), p. 1-5 2. M. I. B. Bernardi, E. J. H. Lee, P. N. Lisboa-Filho, E. R. Leite, E. Longo, J. A. Varela. TiO2 thin film growth using the MOCVD method, Materials Research, 2001, no. 4(3), pp. 1-5

Claims (1)

Procedeu de obţinere a straturilor epitaxiale subţiri de TiO2, care include degresarea unui substrat de sticlă în toluen, uscarea lui în vapori de alcool izopropilic şi plasarea acestuia într-un reactor de depunere chimică din faza de vapori, care se purjează cu argon timp de 20 min cu viteza fluxului de 100 cm3/min, apoi se măreşte temperatura substratului până la 400°C, precum şi producerea vaporilor de izopropoxid de titan prin barbotare la temperatura de 90°C, totodată depunerea straturilor epitaxiale de TiO2 se realizează prin debitarea separată în reactor a vaporilor de izopropoxid de titan, transportaţi cu un flux de argon cu viteza de 40 cm3/min, şi unui flux de oxigen cu viteza de 40 cm3/min, timp de 30 min.Process for obtaining thin epitaxial layers of TiO2, which includes degreasing a glass substrate in toluene, drying it in isopropyl alcohol vapor, and placing it in a chemical vapor deposition reactor, which is purged with argon for 20 min with a flow rate of 100 cm3/min, then the temperature of the substrate is increased up to 400°C, as well as the production of titanium isopropoxide vapors by bubbling at a temperature of 90°C, at the same time the deposition of the epitaxial layers of TiO2 is carried out by separate cutting in reactor of titanium isopropoxide vapors, transported with an argon flow at a speed of 40 cm3/min, and an oxygen flow at a speed of 40 cm3/min, for 30 min.
MDS20230010A 2023-02-02 2023-02-02 Method for producing epitaxial TiO2 thin layers MD1740Z (en)

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MD1740Y MD1740Y (en) 2024-01-31
MD1740Z true MD1740Z (en) 2024-08-31

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