MD712Z - Process for producing MoO3 nanostructures - Google Patents

Process for producing MoO3 nanostructures Download PDF

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Publication number
MD712Z
MD712Z MDS20130058A MDS20130058A MD712Z MD 712 Z MD712 Z MD 712Z MD S20130058 A MDS20130058 A MD S20130058A MD S20130058 A MDS20130058 A MD S20130058A MD 712 Z MD712 Z MD 712Z
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Moldova
Prior art keywords
nanostructures
temperature
moo3
reactor
producing
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MDS20130058A
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Romanian (ro)
Russian (ru)
Inventor
Виорел ТРОФИМ
Олег ЛУПАН
Василий КРЕЦУ
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Технический университет Молдовы
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Priority to MDS20130058A priority Critical patent/MD712Z/en
Publication of MD712Y publication Critical patent/MD712Y/en
Publication of MD712Z publication Critical patent/MD712Z/en

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Abstract

The invention relates to the nanostructured material production technology, in particular to a process for producing molybdenum oxide nanostructures.The process for producing MoO3 nanostructures includes the degreasing of a molybdenum rod, its introduction into a quartz reactor, closed on one side and preheated to a temperature to a temperature of 670…950°C, introduction into the reactor through the quartz tube of distilled water vapors. Nanostructures begin to precipitate on the inner surface of the reactor, to its output, after 10…15 min of maintenance in this zone of the temperature of 420°C.

Description

Invenţia se referă la tehnologia de producere a materialelor nanostructurate, în particular la un procedeu de obţinere a nanostructurilor de oxid de molibden. The invention relates to the technology of producing nanostructured materials, in particular to a process for obtaining molybdenum oxide nanostructures.

Nanostructurile din oxid de molibden sunt folosite pe larg ca senzori de gaze (H2, NH3, NO2, CO), fototranzistori, elemente fotovoltaice. Molybdenum oxide nanostructures are widely used as gas sensors (H2, NH3, NO2, CO), phototransistors, and photovoltaic elements.

Este cunoscut un procedeu de obţinere a nanobaghetelor de MoO3 din soluţia de MoO3·2H2O prin metoda solvotermală. Tratarea are loc în apă la o temperatură de 180°С, într-un mediu acid şi timp de la câteva ore până la 7 zile [1]. A process for obtaining MoO3 nanorods from MoO3·2H2O solution by the solvothermal method is known. The treatment takes place in water at a temperature of 180°С, in an acidic environment and for a period of several hours to 7 days [1].

Dezavantajul acestui procedeu este timpul îndelungat de creştere a acestor nanostructuri. The disadvantage of this process is the long growth time of these nanostructures.

Este cunoscut, de asemenea, procedeul de obţinere a nanostructurilor prin încălzirea directă a spiralei de Mo în atmosferă. Datorită trecerii curenţilor de 25, 50, 75 A, spirala se încălzeşte până la temperaturile de 700, 1000, 1300°C, respectiv. Depunerea nanostructurilor are loc pe o plachetă din Si, încălzită până la 200°C, plasată la 5 cm de spirală [2]. The process of obtaining nanostructures by direct heating of the Mo spiral in the atmosphere is also known. Due to the passage of currents of 25, 50, 75 A, the spiral heats up to temperatures of 700, 1000, 1300°C, respectively. The deposition of nanostructures takes place on a Si wafer, heated to 200°C, placed 5 cm from the spiral [2].

Dezavantajul acestui procedeu este temperatura înaltă a procesului. Dezavantajul ambelor procedee constă în imposibilitatea de reglare a dimensiunilor nanostructurilor. The disadvantage of this process is the high process temperature. The disadvantage of both processes is the impossibility of adjusting the dimensions of the nanostructures.

Cea mai apropiată soluţie este procedeul de obţinere a structurilor de MoO3, care constă în încălzirea unei plăci de molibden la temperatura de 1000…1080°C într-un tub de cuarţ direct în aer. Nanostructurile se obţin în regiunea tubului de cuarţ cu temperatura de 360…380°C. Timpul de creştere este între 0,5 şi 24 ore [3]. The closest solution is the process of obtaining MoO3 structures, which consists of heating a molybdenum plate at a temperature of 1000…1080°C in a quartz tube directly in air. Nanostructures are obtained in the region of the quartz tube with a temperature of 360…380°C. The growth time is between 0.5 and 24 hours [3].

Dezavantajul acestui procedeu este temperatura înaltă în cuptor în timpul creşterii. The disadvantage of this process is the high temperature in the oven during rising.

Problema pe care o rezolvă invenţia propusă constă în obţinerea nanostructurilor de MoO3 prin oxidarea termică rapidă în vapori de apă a tijei de molibden la temperaturi relativ mici şi timpul redus. The problem solved by the proposed invention consists in obtaining MoO3 nanostructures by rapid thermal oxidation of the molybdenum rod in water vapor at relatively low temperatures and in a short time.

Procedeul, conform invenţiei, înlătură dezavantajele menţionate mai sus prin aceea că include degresarea unei tije de molibden, introducerea ei într-un reactor de cuarţ, închis dintr-o parte şi încălzit preventiv până la o temperatură de 670...950°C, introducerea în reactor printr-un tub de cuarţ a vaporilor de apă distilată. Nanostructurile încep a se depune pe suprafaţa interioară a reactorului, la ieşirea lui, după 10...15 min de menţinere în această zonă a temperaturii de 420°C. The process, according to the invention, eliminates the above-mentioned disadvantages by including the degreasing of a molybdenum rod, its introduction into a quartz reactor, closed on one side and preheated to a temperature of 670...950°C, the introduction into the reactor through a quartz tube of distilled water vapor. Nanostructures begin to deposit on the inner surface of the reactor, at its outlet, after 10...15 min of maintaining the temperature of 420°C in this area.

Rezultatul invenţiei constă în obţinerea nanostructurilor de MoO3. Cantitatea nanostructurilor depinde de timpul procesului, iar dimensiunile maximale depind de temperatura procesului. The result of the invention consists in obtaining MoO3 nanostructures. The quantity of nanostructures depends on the process time, and the maximum dimensions depend on the process temperature.

Procesul de creştere a nanostructurilor a avut loc în intervalul de temperaturi 670…950°C şi timp de 10…15 min. The nanostructure growth process took place in the temperature range of 670…950°C and for 10…15 min.

Invenţia se explică prin imaginile reprezentate în fig. 1 - 4, care reprezintă componenţa chimică a nanostructurilor MoO3 şi imaginile fotografice ale nanostructurilor, obţinute la diferite temperaturi şi intervale de timp, realizate cu un microscop electric la scanarea lor: The invention is explained by the images represented in Fig. 1 - 4, which represent the chemical composition of MoO3 nanostructures and the photographic images of the nanostructures, obtained at different temperatures and time intervals, made with an electric microscope when scanning them:

- fig. 1, componenţa chimică a nanostructurilor MoO3; - Fig. 1, chemical composition of MoO3 nanostructures;

- fig. 2, imaginea nanostructurilor obţinute la temperatura de 670°C şi t = 15 min; - Fig. 2, image of nanostructures obtained at a temperature of 670°C and t = 15 min;

- fig. 3, imaginea nanostructurilor obţinute la temperatura de 800°C şi t = 15 min; - Fig. 3, image of nanostructures obtained at a temperature of 800°C and t = 15 min;

- fig. 4, imaginea nanostructurilor obţinute la temperatura de 900°C şi t = 10 min. - Fig. 4, image of nanostructures obtained at a temperature of 900°C and t = 10 min.

Exemplu de realizare Example of implementation

O tijă din molibden cu diametrul de 3 mm cu puritatea 99,8% a fost degresată în toluen marca CPA, apoi spălată în apă distilată. Tija din molibden a fost introdusă în reactorul din cuarţ închis dintr-o parte, prealabil încălzit într-un cuptor electric industrial (CDO-125/4) până la temperatura minimală de 670°C. A 3 mm diameter molybdenum rod with 99.8% purity was degreased in CPA brand toluene, then washed in distilled water. The molybdenum rod was inserted into the quartz reactor closed on one side, previously heated in an industrial electric furnace (CDO-125/4) to a minimum temperature of 670°C.

Printr-un tub de cuarţ cu diametrul de 8…10 mm au fost introduşi în reactor vapori de apă distilată dintr-un barbotor, unde apa fierbea. Presiunea vaporilor saturaţi era de aproximativ 1 atm. Distilled water vapor from a bubbler, where the water was boiling, was introduced into the reactor through a quartz tube with a diameter of 8…10 mm. The saturated vapor pressure was approximately 1 atm.

Ca rezultat al reacţiei chimice dintre molibden şi vaporii de apă s-au format vapori din MoO3, care se mişcau spre ieşirea din reactor. Pe suprafaţa reactorului la temperatura de 420°C s-au format nanostructurile de MoO3. Compoziţia nanostructurilor de MoO3 a fost monitorizată prin analiza spectrogramei de dispersie energetică a razelor X (EDX) înregistrate de un spectrometru (Oxford Instrument Analytical), ataşat la un microscop electric VEGA TS5130MM (fig. 1). As a result of the chemical reaction between molybdenum and water vapor, MoO3 vapors were formed, which moved towards the reactor outlet. MoO3 nanostructures were formed on the reactor surface at a temperature of 420°C. The composition of the MoO3 nanostructures was monitored by analyzing the energy dispersive X-ray (EDX) spectrogram recorded by a spectrometer (Oxford Instrument Analytical) attached to a VEGA TS5130MM electron microscope (Fig. 1).

1. Greta R. Patzke, Alexej Michailovski, Frank Krumeich and etc. One-Step Synthesis of Submicrometer Fibers of MoO3, Chem. Mater., 2004, 16 (6), p. 1126-1134 1. Greta R. Patzke, Alexej Michailovski, Frank Krumeich and etc. One-Step Synthesis of Submicrometer Fibers of MoO3, Chem. Mater., 2004, 16 (6), p. 1126-1134

2. Ye Zhao, Jingguo Liu, Ya Zhou, Zhengjun Zhang and etc. Preparation of MoO3 nanostructures and their optical 2. Ye Zhao, Jingguo Liu, Ya Zhou, Zhengjun Zhang and etc. Preparation of MoO3 nanostructures and their optical

properties. J. Phys.: Condens. Matter, 2003, V. 15 L547-L552 properties. J. Phys.: Condens. Matter, 2003, V. 15 L547-L552

3. Petre Badica. Preparation through the Vapor Transport and Growth Mechanism of the First-Order Hierarchical Structures of MoO3 Belts on Sillimanite Fibers, Crystal Growth & Design, 2007, V. 7 (4), p. 794-801 3. Petre Badica. Preparation through the Vapor Transport and Growth Mechanism of the First-Order Hierarchical Structures of MoO3 Belts on Sillimanite Fibers, Crystal Growth & Design, 2007, V. 7 (4), p. 794-801

Claims (1)

Procedeu de obţinere a nanostructurilor de MoO3, care include degresarea unei tije de molibden, introducerea ei într-un reactor de cuarţ, închis dintr-o parte şi încălzit preventiv până la o temperatură de 670...950°C, introducerea în reactor printr-un tub de cuarţ a vaporilor de apă distilată, iar nanostructurile încep a se depune pe suprafaţa interioară a reactorului, la ieşirea lui, după 10...15 min de menţinere în această zonă a temperaturii de 420°C.Process for obtaining MoO3 nanostructures, which includes degreasing a molybdenum rod, introducing it into a quartz reactor, closed on one side and preheated to a temperature of 670...950°C, introducing distilled water vapor into the reactor through a quartz tube, and the nanostructures begin to deposit on the inner surface of the reactor, at its exit, after 10...15 min of maintaining the temperature of 420°C in this area.
MDS20130058A 2013-03-26 2013-03-26 Process for producing MoO3 nanostructures MD712Z (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
MD4347C1 (en) * 2014-07-15 2015-11-30 Виорел ТРОФИМ Gas sensor based on MoO3
CN105948122A (en) * 2016-04-29 2016-09-21 中南大学 Method for preparing high-purity molybdenum trioxide
  • 2013

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
Greta R. Patzke, Alexej Michailovski, Frank Krumeich and etc. One-Step Synthesis of Submicrometer Fibers of MoO3, Chem. Mater., 2004, 16 (6), p. 1126–1134 *
Petre Badica. Preparation through the Vapor Transport and Growth Mechanism of the First-Order Hierarchical Structures of MoO3 Belts on Sillimanite Fibers, Crystal Growth & Design, 2007, V. 7 (4), p. 794-801 *
Ye Zhao, Jingguo Liu, Ya Zhou, Zhengjun Zhang and etc. Preparation of MoO3 nanostructures and their optical properties. J. Phys.: Condens. Matter, 2003, V. 15 L547-L552 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
MD4347C1 (en) * 2014-07-15 2015-11-30 Виорел ТРОФИМ Gas sensor based on MoO3
CN105948122A (en) * 2016-04-29 2016-09-21 中南大学 Method for preparing high-purity molybdenum trioxide
CN105948122B (en) * 2016-04-29 2017-06-06 中南大学 A kind of method for preparing high-purity molybdenum trioxide

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