RU2138440C1 - Device for synthesis of fluorine-derivative fullerens - Google Patents

Abstract

FIELD: vacuum engineering. SUBSTANCE: device presents evaporator of mass spectrometer including cooling jacket, cover, holder of effusive cell, resistance furnace located round effusive cell and thermocouple, soldered to lower base of cell. Distinguishing feature of device is presence in evaporator cover of collecting plate made of metal resistant to fluorine and having hole coaxial to holes in effusive cell and evaporator cover. Fluorination products are formed in effusive cell and fly out of cell to be condensed on cold collecting plate and partially get through existent hole to ionization chamber of mass spectrometer. Thus, mass-spectral control of synthesis is effected. Upon completion of synthesis, collecting plate is separated and substance is easily collected. EFFECT: constant mass-spectral control of synthesis process and increased product yield. 1 dwg

Description

 The invention relates to vacuum technology.

 A device [1] is known for producing fluorine derivatives of fullerenes, which includes an effusion cell of a mass spectrometer with an inlet of a fluorinating agent. Closest to the proposed device is the work [2], which is also an evaporator of the ion source of the mass spectrometer, which includes an effusion cell with the reaction mixture in it, a cell holder, a resistance furnace, a cooling jacket, a thermocouple welded to the bottom cell base, and cover. The resistance furnace is pressed against the cell holder by means of a screen (a sheet metal cylinder without bases), the side surfaces of which touch the holder through ceramic insulators. Behind the evaporator are an ionization device with electrodes, a mass analyzer and an ion detector. The known device does not allow to sufficiently collect the resulting fluorination products. The yield is ≈ 5%.

 Problem to be solved: creation of a device for the synthesis of fluorine derivatives of fullerenes, which allows to increase the final product yield.

 The problem is achieved by the proposed device for the synthesis of fluorine derivatives of fullerenes, containing a mass spectrometer evaporator, including a jacket, a cooling evaporator, a cover designed to protect the mass spectrometer ionizer and equipped with a collecting plate made of fluorine-resistant metal located on the inside of the evaporator and having an opening, coaxial with holes in the effusion cell and the lid of the evaporator; holder of the effusion cell in which the effusion cell with the reaction esyu, resistance furnace disposed around the cell, and a thermocouple welded to the lower base of the cell.

 The difference of the proposed device is that the evaporator lid is equipped with a collecting plate made of fluorine-resistant metal located on the inside of the evaporator and having a hole coaxial with the holes in the effusion cell and the lid of the evaporator.

 The drawing shows a diagram of the device, which shows: 1 - effusion cell, 2 - reaction mixture, 3 - cell holder, 4 - evaporator cover, 5 - collecting plate made of fluorine-resistant material, 6 - cooling water jacket, 7 - resistance furnace, 8 - thermocouple. The screen pressing the furnace is not indicated on the diagram.

 The inventive device for the synthesis of fluorine derivatives of fullerenes by the interaction of fullerenes with transition metal fluorides is a mass spectrometer evaporator, which includes a jacket (6), a cooling evaporator, a cover (4) designed to protect the mass spectrometer ionizer, and equipped with a collecting plate (5 ) made of fluorine-resistant metal located on the inside of the evaporator and having a hole coaxial with the holes in the effusion cell and the evaporator cap, holder of the effusion cell ki (3), wherein the fixed effusion cell (1) with the reaction mixture (2), resistance furnace (7), arranged around the cell and concerning its through ceramic insulators, and a thermocouple (8) is welded to the lower base of the cell.

 In the effusion cell (1) is placed the reaction mixture (2), consisting of fullerene and a fluorinating agent (transition metal fluoride), upon heating of which the formation of fluorination products, which are more volatile than the starting materials, and escaping from it. Then they condense on a cold collecting plate (5), and a small part of them flies out through the hole in it into the ionization chamber of the mass spectrometer (not shown in the diagram). Thus, mass spectral control of the synthesis is carried out. After completion of the synthesis, the plate (5) can be separated, and the substance can be easily collected. The yield is ≈ 40%.

 The technical result of the proposed invention is constant mass spectrometric monitoring of the efficiency and selectivity of the synthesis process, allowing you to choose the optimal synthesis temperature, and increase the final product yield due to the presence of a collecting plate.

Literature
[1] A.S. Alikhanyan, I.N.Malkerova, D.V. Sevastyanov, S.P. Ionov, V.F. Sukhoverkhov, N.G. Spitsyna Journal of Inorganic Chemistry, 1995, 40, 1502-1509.

 [2] O. V. Boltalina, A. Ya. Borschevskii, L. N. Sidorov, J. M. Street, R. Taylor. J. Chem. Soc. Chem. Commun. 1996 529-530f

Claims (1)

 A device for synthesizing fluorine derivatives of fullerenes, comprising a mass spectrometer evaporator, including a jacket, a cooling evaporator, a cover for protecting the mass spectrometer ionizer, an effusion cell holder in which an effusion cell with a reaction mixture is fixed, a resistance furnace located around the cell, and a thermocouple welded to the lower base of the cell, characterized in that the evaporator cap is equipped with a collecting plate made of fluorine-resistant metal and having an opening coaxial suspended with holes in the effusion cell and evaporator cap.