Polyfluorinated diminati metals as precursors for the metallization of various solid surfaces and to obtain metallic mirrors

 

(57) Abstract:

The invention concerns new compounds of polyfluorinated deimination metals of the formula I, in which RFis a CF3C2F5and C4F9M represents Fe(III), Co(II), Ni, cu, Zn; n is 2 or 3; provided that when RFis a CF3, M cannot be a Co(II), Ni, cu, Zn. The new compounds possess high stability, good solubility in almost all organic solvents and can be used as precursors for the metallization of various surfaces, including the obtaining of metallic mirrors. 1 PL.

The invention relates to the field of organic chemistry, specifically to provide new compounds of polyfluorinated deimination metals General formula:

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where RFis a CF3C2F5C4F9; M is Fe(III), Co(II), Ni, Cu; n is an integer equal to 2 or 3; provided that when RFis a CF3, M cannot be a Co(II), Ni, Cu, Zn.

Polyfluorinated diminati metals can be used as precursors for metallicatv literature are not described.

The complex hexafluoroacetylacetonate copper(I) vinyltrimethylsilane (Cu(I)(hfaa)(VTMS)), which is used to obtain a copper film. However, this compound is easily decomposed at temperatures above 40oC and slowly decomposes even at room temperature. [2, Appl. Phys. Lett. 1993, 63, 2842].

Also known complex hexafluoroacetylacetonate copper(I) VINYLTRIMETHOXYSILANE (Cu(I)(hfaa)(VMOS)). Upon receipt of the copper film authors use expensive solvents (laterobasal), the process is conducted under pressure, in an argon atmosphere [1, Appl. Phys. Lett. 1996, 68, 1017].

Known salt of divalent copper hexafluoroacetylacetonate copper(II) (Cu(hfaa)2), however, the presence in the molecule directly associated copper - oxygen entails the complexity of the process for obtaining metallic film (the use of combustible gas (hydrogen)) [3, Appl. Phys. Lett. 1992, 61, 2175].

The objective of the invention is to provide new compounds with increased stability, good solubility in almost all organic solvents which can be used as precursors for the metallization of various solid surfaces, and including to obtain metal A formula

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acetate or acetylacetonate of a suitable metal in an open system, in an organic solvent.

The reaction is carried out according to the following scheme:

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Mass spectra were recorded on a mass spectrometer "Kratos MS-890" (ionizing voltage 70 eV).

Example 1. To aqueous solution of 0.36 g of basic acetate of iron(III) add 1,2 2-amino-4-aminopropiophenone-2 in 20 ml of ether. The reaction mixture is stirred for 1 h to Separate the organic layer. The solvent is evaporated, the solid residue is recrystallized from CCl4. Received 0,70 g (54%) iron(III) - Tris(1,1,1,3,5,5,5-heptathlon-2-aminoindan-2-amine-4-ATA) in the form of crystals brown-green color. MP. 167 - 170oC, (M+m/z 725).

Found, %: C 25,21; H 0,78; Fe 7,83; N TO 11.56

C15H6F21FeN6< / BR>
Calculated, %: C 24,83; H 0,82; Fe 7,72; N 11,59

Example 2. To 0.65 g acetylacetonate cobalt (II) was added 1.0 g of 2-amino-4-aminopropiophenone-2 in 20 ml of ether. The organic layer is separated. The solvent is evaporated, the solid residue is recrystallized from CCl4. Obtained 0.75 g (67%) epirate cobalt(II) bis(1,1,1,3,5,5,5-heptathlon-2-aminoindan-2-amine-4-ATA) in the form of crystals of red-brown color. MP. 135 - 137oC, (M+m/z 505).

Nai>Example 3. Similar to the above from 0,59 g of zinc acetylacetonate and 1.0 g of 2-amino-4-aminopropiophenone-2 was obtained 0,60 g (53%) zinc-bis-(1,1,1,3,5,5,5-heptathlon-2-aminoindan-2-amine-4-ATA) in the form of crystals of pale yellow color. MP. 220 - 224oC, (M+m/z 511).

Found, %: C 23,96; H 0,83; N OF 11.15

C10F14ZnN4< / BR>
Calculated, %: C 23,48; H 0,78; N 10,96

Example 4. To 0,22 g of copper acetate was added 0.5 g of 2-amino-4-aminopropiophenone-2 in 20 ml of acetone. The solvent is evaporated, the solid residue is recrystallized from CCl4. Received 0,30 g (53%) copper-bis-(1,1,1,3,5,5,5-heptathlon-2-aminoindan-2-amine-4-ATA) in the form of crystals of dark green color. MP. 162 - 167oC, (M+m/z 510).

Found, %: C 23,66; H 0,57; Cu 10,97; N 10,91

C10H4F14CuN4< / BR>
Calculated, %: C 11,72; C 23,53,; H 0,78; N 10,98

Example 5. Similar to the above from 0,57 g of Nickel acetate and 1.0 g of 2-amino-4-aminopropiophenone-2 was obtained of 0.53 g (54%) epirate Nickel bis(1,1,1,3,5,5,5-heptathlon-2-aminoindan-2-amine-4-ATA) in the form of crystals of dark green color. MP. 176 - 180oC, (M+m/z 505).

Found, %: C 30,67; H 2,24; Ni 9,11; N 9,52

C14H14F14NiN4O

Calculated, %: C 29,09; H 2,42; Ni 10,18; N 9,67

Example 6. Similarly opisane-2-aminohexyl-2-amine-4-ATA) in the form of crystals of dark green color. MP. 114 - 118oC.

Found, %: C 23,51; H 0,36; Cu 9,43; N 9,26

C12H4F18CuN4< / BR>
Calculated, %: C 23,68; H 0,33; Cu 10,52; N OF 9.21

Example 7. To aqueous solution of 2.2 g of copper acetate was added 4.5 g of 2-amino-4-aminopropiophenone-2 in 20 ml of ether. The reaction mixture is stirred for 1 h to Separate the organic layer. The solvent is evaporated, the solid residue is recrystallized from CCl4. Received of 5.2 g (71%) copper-bis-(1,1,1,3,5,5,6,6,7,7,8,8,8-dogcatcher-2-aminooctane-2-amine-4-ATA) as dark green crystals. MP. 79 - 83oC.

Found, %: C 26,60; H 0,56; Cu 8,56; N 7,72

C16H4F26CuN4< / BR>
Calculated, %: C 26,75; H 0,54; Cu 8,7; N 7,6

The metal film obtained by applying diminuta suitable metal dissolved in an organic solvent, onto a solid surface followed by heating.

The stability of the proposed deimination metals was evaluated using mass spectroscopy (mass spectra observed molecular ion), thermogravimetry (substances which melt without decomposition, the total mass loss is 91-100%), elemental analysis (elemental analysis data diminuta copper, which was kept for 5 years under normal conditions coincide with data elementaries polyfluorinated diminati metals have a high stability, good solubility in almost all organic solvents. The results show that the inventive compounds may be used as precursors for the metallization of various solid surfaces, including the obtaining of metallic mirrors, as it does not require the use of expensive and hard-to-reach solvents and combustible gas (hydrogen).

There is the act of testing individual parts of rolling bearings and plain bearings coated with a coating made of diminuta copper. There is reason to judge the increased durability of the bearings without reducing their vibroacoustic characteristics (see table).

Polyfluorinated diminati metals of the formula I:

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where RFis a CF3C2F5C4F9;

M is Fe(III), Co(II), Ni, Cu, Zn;

n is an integer equal to 2 or 3, provided that when RFis a CF3, M cannot be a Co(II), Ni, Cu, Zn;

as precursors for the metallization of various solid surfaces and to obtain metallic mirrors.

 

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