Luminescent semiconductor polymer material and a method for preparation thereof

FIELD: polymer materials.

SUBSTANCE: invention provides luminescent material showing semiconductor properties and being product of complex polymerization in glow discharge, which is formed as a supported polymer layer located either between electrodes or on any of electrodes. Starting pyrromethene complex is difluoroborate complex of 1,3,5,7,8-pentamethyl-2,6-diethylpyrromethene (Pyrromethene 567). Method of preparing luminescent semiconductor polymer material comprises glow-discharge polymerization for 2 to 120 min of Pyrromethene 567 vapors at temperature preferably 250-350°C, pressure 10-1 to 10-2 Pa, and discharge power 0.5-3 W. Resulting luminescent polymer is characterized by thickness preferably 0.001-10 μm, conductivity 1·10-10 to 5·10-10 Ohm-1cm-1 (20°C), luminescence emission maximum in the region of 540-585 nm at band halfwidth 55-75 nm. Polymer is obtained with quantum yield 0.6-0.8 and is designed for creation of film light-emitting devices.

EFFECT: improved performance characteristics of material.

13 cl, 3 ex

 

The technical field

The invention relates to the field of light-emitting material, which can be used to create light-emitting devices and devices that will luminesce when photo - or elektrovojvodina. More specifically the invention relates to luminescent semiconducting material on the basis of pyrromethene complex, in particular, obtained by polymerization in a glow discharge. The invention relates also to a method for producing semi-conducting luminescent material based pyrromethene complex.

The level of technology

Known electroluminescent materials based on bis-(2-oxybenzone-4-tertbutylamine)-zinc and fluorescent additives such as dye Nile red, present in an amount of from 0.1 to 5 wt.% (patent RF №2155204, publ. 27.08.2000). Such materials emit in the red region of the spectrum (approximately 632 nm). Their disadvantage is the lack of mechanical strength. This is because this material is a mixture of two low molecular weight substances.

In addition, the known luminescent materials consisting of organic semi-conducting component and the phosphor and capable of electroluminescence (Japan patent No. JP 9082473, publ. 28.03.1997; and publication of a European patent application no EP 669387, publ. 30.08.1995). A common shortcoming of such mA the materials is the presence in the spectrum of emission in addition to the strips, associated with phosphor, unwanted bands associated with the semiconductor component.

Next, a known fluorescent organosilicon polymer materials and methods for producing these materials (U.S. patent No. 6361885, publ. 26.03.2002). Part of the main polymer chain is attached through covalent bonds of organic component that has the ability to luminescence and consisting of two or more condensed aromatic rings containing substituents. Light-emitting polymer according to this patent is obtained by the resultant deposition rates 9,10-bis-(3-trichlorosilyl)-anthracene, synthesized by a multi-stage method, the glass substrate at a high temperature and a residual pressure of about 10-6Torr. Next presidency layer kept in air for 15 min, then heated at a temperature of approximately 110°C for about 30 minutes the resulting polymer has a weak light purple fluorescent glow in the range from about 370 to about 430 nm. The main disadvantages of these luminescent polymer materials are complex, multi-stage method of obtaining the source of the monomer and the polymer, and the low intensity of the glow.

Also known luminescent polymers containing repeating aralen-vinylene the e fragments and fluorinated tetraphenyl fragments. These materials are obtained by copolymerization of fluorinated tetraphenyl derived from the MDA, which consists of two allenbyi group (U.S. patent No. 6495273, publ. 17.12.2002). Obtaining fluorinated tetraphenylboron derived monomer conduct of specially synthesized 1,22-bis-(methyl bromide)-8,9,11,12,14,15,17,18-octafluorotoluene in the presence of triphenylphosphine. Light-emitting polymer material is produced by the interaction of the specified monomer with arlindialede.html in which allenbyi group may include, for example, thiophene, phenyl, and carbazole. Thin film electroluminescence is obtained from the solution using the method of spin casting. The area of the luminescence of this material ranges from about 250 to about 490 nm. The disadvantages of these materials are the inaccessibility of the parent compounds, as well as the need for additional stages remove traces of catalyst and solvent.

Most similar in composition to the claimed fluorescent material are light-emitting materials based on derivatives dicaterino(3,4-C)pyrrole, which include pyrometry complex (publication of the patent application U.S. No. 2003/0082406 A1, publ. 01.05.2003). Used in this case derived dicaterino(3,4-C)pyrrole have different alkyl substituents with h the scrapping of the carbon atoms in the range from about 1 to about 25, moreover, these derivatives are not polymers. Pyrometry complex type to derived dicaterino(3,4-C)pyrrole in an amount of from about 0.1 wt.% to about 1 wt.%. The luminescence of the material obtained is in the yellow-red region (from about 580 to about 720 nm). The disadvantage of these fluorescent materials is inaccessibility derivatives dicaterino(3,4-C)pyrrole. In addition, due to the low molecular weight organic material does not provide good mechanical strength in the form of a luminescent layer.

The closest to the technical nature of the claimed method for producing a luminescent polymer material is a method of obtaining a fluorescent material on the basis of 3-hydroxyflavone, the radiation of which is in the range of from about 375 to about 475 nm by RF magnetron sputtering from the surface of an aluminium target in a stream of carrier gas which is a mixture of approximately 95% Ar and about 5% O2(G. Maggioni, S. Carturan, A, Quaranta, A. Patelli, G. Delia Mea, V. Rigato // Surface and Coatings Technology, 2003, V.174-175, p.1151-1158). This process is carried out in a high-frequency (about 13.56 MHz) discharge high power (about 600 watts) with pre-pumping reaction chamber to about 10-5PA, placing the powder 3-hydroxyflavone on target for magnets is spent spraying. When spraying the dye used capacity of at least 10-30 watts. However, the use of so much power, as can be seen from the mass spectra of the gas phase formed in the process of obtaining material, leads to the partial degradation of 3-hydroxyflavone. The disadvantages of this method are that the resulting luminescent material is unstable in storage, and the deterioration of the emission properties observed after finding material on the air for several hours. In addition, the light-emitting material also varies appearance: initially dense and uniform film becomes loose and powdery. In addition, the disadvantages of this method are very energy intensive process, high working frequency (about 13.56 MHz), which in an industrial variant of tools should be used to special protection personnel. Another drawback is the necessity of using special carrier gas (argon).

Disclosure of inventions

The present invention is the creation of a luminescent polymer material in the form of a thin mechanically strong polymer layer. The luminescent material according to the present invention has a greater intensity of radiation in the green-yellow spectral region and has a conductivity that is necessary is for the electroluminescence. The present invention is the creation of the fluorescent polymer based material commercially available starting compounds of the phosphor. The present invention is also a method that allows to obtain a luminescent polymeric material that has a conductivity sufficient to electroluminescence from a single commercially available starting compounds of the phosphor without any substantial change in its fluorescent properties. In addition, the present invention is the obtaining of such material in the form of a solid polymer film with varied over a wide range of thickness.

According to one aspect of the present invention proposed a luminescent material based on pyrromethene complex, having semi-conducting properties and which is the product of polymerization pyrromethene complex in glow discharge obtained in the form of a polymer layer on a substrate placed between the electrodes or on any of the electrodes.

In one of specific embodiments pyrometry complex can be deformity complex 1,3,5,7,8-pentamethyl-2,6-diarylpyrimidine (pyrromethene 567). The maximum luminescence of this material is observed in the yellow-green region of the spectrum in the range from 540 to 585 nm, pricenausea strip is in the range from 55 to 75 nm, and quantum yield of photoluminescence is in the range from 0.6 to 0.8. The fluorescent material can be obtained in the form of a polymer layer with a thickness in the range from 0.01 to 10 μm and has an electrical conductivity at a temperature of 20°C in the range from 1·10-10up to 5·10-10Ω-1·cm-1. Polymerization in a glow discharge can be carried out at a temperature in the range from 250 to 350°C, at a residual pressure in the range of 10-1up to 10-2PA, when the discharge power in the range from 0.5 to 3 W, and during the residence time in the range from 2 to 120 minutes. The luminescent material may be deposited on a substrate in a glow discharge. In one specific embodiment, the substrate may be made for example of metal, dielectric material or semiconductor material with a conductive coating.

Semi-conducting luminescent material according to the present invention receive a special way. Pair pyrromethene complex can be polymerized in a glow discharge with the formation of a polymeric layer on a substrate placed between the electrodes or on any of the electrodes. In particular, the luminescent material according to the present invention can be obtained by polymerization difibulator complex 1,3,5,7,8-pentamethyl-2,6-diarylpyrimidine (pyrromethene 567) the glow discharge at a temperature in the range from 250 to 350° C, at a pressure in the range of 10-1up to 10-2PA and the discharge power in the range from 0.5 to 3 watts. The resulting product may be precipitated on a substrate placed between the electrodes or on any of the electrodes. Material capable of luminescence in the yellow-green region of the spectrum with a maximum in the region from 540 to 585 nm, with full width at half maximum of the emission band in the range from 55 to 75 nm and quantum yield of photoluminescence in the range from 0.6 to 0.8. In one particular embodiment, the polymeric layer may have a thickness in the range from 0.01 to 10-10m Thickness of this layer depends on the duration of the polymerization process in a glow discharge, which may correspond to a time period in the range from 2 to 120 minutes. The polymer may have a conductivity at room temperature in the range from 1·10-10up to 5·10-10Ω-1·cm-1.

According to another aspect of the present invention, a method for obtaining a fluorescent material according to any one of items 1 to 8, comprising the polymerization of vapor pyrromethene complex in the glow discharge at low pressure and temperature, providing the necessary vapor pressure, in a period of time sufficient for formation of a polymer layer of the required thickness on a substrate placed between the electrodes or on any of the electrodes.

<> In one specific embodiment, as pyrromethene complex use deformity complex 1,3,5,7,8-pentamethyl-2,6-diarylpyrimidine (pyrromethene 567). The polymerization process can be carried out at a temperature in the range from 250 to 350°C, at a residual pressure in the range of 10-1up to 10-2PA, a discharge power in the range from 0.5 to 3 W and for a period of time ranging from 2 to 120 minutes. The substrate can be used, for example, a metal, a dielectric material or a semiconductor material with a conductive coating.

The obtained luminescent material is intended to create a film of polymer light-emitting devices.

The polymer material according to the present invention has the ability to luminescence due to the fact that polymerization occurs in a glow discharge at low values of discharge power, do not cause any significant changes in the chemical structure of a molecule difibulator complex 1,3,5,7,8-pentamethyl-2,6-diarylpyrimidine (pyrromethene 567).

Brief description of drawings

Figure 1 is a graph illustrating the absorption spectrum and the luminescence spectrum of source materials, i.e. dissolved in ethanol difibulator complex 1,3,5,7,8-pentamethyl-2,6-diarylpyrimidine (pyrromethene 567), and SPECT the absorption and the luminescence spectrum of the fluorescent polymer according to the present invention.

Figure 2 is a representation in cross-section, showing the luminescent polymer according to the variant embodiment of the invention, located on the made of quartz glass substrate.

Referring to figure 1, it is seen that the resulting polymer has the luminescence spectrum (curve IIa), similar to the spectrum of the luminescence curve (Ia) molecular solution of starting compound - difibulator complex 1,3,5,7,8-pentamethyl-2,6-diarylpyrimidine. The band maxima of the luminescence of the parent compound and the polymer material on the basis of this initial compounds correspond to each other and are in the wavelength range from 540 to 542 nm. Half-band luminescence of the polymer material is in the range from 55 to 60 nm. Absorption spectrum (curve II) a polymer-based material difibulator complex 1,3,5,7,8-pentamethyl-2,6-diarylpyrimidine shows a slight shift to shorter wavelengths relative to the absorption spectrum (curve I) solution of the original substance in ethanol (maxima occur at 500 nm and 520 nm, respectively). All this suggests that in the elementary level obtained polymer material stored chemical structure of the parent compound and the configuration of its energy levels. Source deformity complex 1,3,5,7,8-pentam the Teal-2,6-diarylpyrimidine (pyrromethene 567) has a crystalline structure and is soluble in organic solvents, such as, for example, ethyl alcohol and chloroform. Morphological structure obtained according to the present invention a light-emitting polymer is substantially different from the original substance, which is confirmed by the absence of a crystalline phase in the polymer samples in their study using optical microscopy in polarized light. The resulting polymer is not soluble in organic solvents, such as, for example, ethyl alcohol and chloroform.

Referring to figure 2, which illustrates one of the embodiments of the present invention, the polymer forms a continuous homogeneous layer and has good adhesion to the substrate (i.e. withstand the Scotch tape test). The data suggests that the fluorescent polymeric material according to the present invention retains the functional structural elements responsible for the expression of fluorescent properties. In addition, the obtained luminescent polymeric material has a semi-conducting properties, such as conductivity at 20°C in the range from 1·10-10up to 5·10-10Ω-1·cm-1.

In one of the embodiments obtaining the luminescent polymeric material by polymerization in a glow discharge is conducted with the setup described, for example, in the patent of Russian Federation №2205838, publ. 10.06.203 (see figure 3 of the patent). In this case, the reaction chamber may be provided with two plane-parallel electrodes. On one of the electrodes may be placed in the Cup of the original substance. The upper part of the reaction chamber is placed in an electric furnace, which heats the reaction chamber to the required temperature, which is controlled using a thermocouple chromel-Copel. Before carrying out the polymerization process and polymer deposition layer on a substrate placed between the electrodes or on any of the electrodes, the reaction chamber is initially vacuum to a residual pressure of not more than about 10-3PA. Then the chamber is heated to the desired temperature, served on the electrode voltage glow discharge and carry out the polymerization in a glow discharge.

EXAMPLES

Specific Example 1

Polymerization difibulator complex 1,3,5,7,8-pentamethyl-2,6-diarylpyrimidine (pyrromethene 567) were carried out in a glow discharge at a temperature of approximately 250°C, when the discharge power of about 0.5 W and a residual pressure of about 10-2PA for about 2 minutes. The polymer layer was besieged on a substrate made of quartz glass coated with a conductive coating and placed on one of the electrodes. The formed layer had a thickness of about 0.01 µm, the conductivity is approximately 1·1010 Ω-1·cm-1maximum luminescence in the spectral range from 540 to 544 nm at the half-width of luminescence band in the range from 55 to 60 nm with a quantum yield of photoluminescence about 0.8.

Specific Example 2

The layer of the luminescent polymeric material was prepared analogously to Example 1, but with the following process conditions. The polymerization was carried out at a temperature of approximately 350°C, the discharge power was approximately 3 watts, the residual pressure was approximately 10-1PA, and the residence time was approximately 120 minutes. The formed layer was besieged on a substrate of silicon, is placed on one of the electrodes, and this layer has a thickness of approximately 10 μm, the electrical conductivity of about 5·10-10Ω-1·cm-1maximum luminescence in the spectral range from 575 to 585 nm when the half-width of luminescence band in the range from 65 to 75 nm with a quantum yield of photoluminescence approximately 0.6.

Specific Example 3

The layer of the luminescent polymeric material was prepared analogously to Example 1, but with the following process conditions. The polymerization was carried out at a temperature of about 300°C, when the discharge power of about 1.5 watts, at a residual pressure of approximately 5·10-2PA and duration of polymerization in about 60 minutes. Forming the layer besieged on a substrate of metal, placed between the electrodes, and the layer had a thickness of about 5 μm, the electrical conductivity of approximately 2·10-10Ω-1·cm-1maximum luminescence in the spectral range from 560 to 570 nm at the half-width of luminescence band in the range from 60 to 65 nm with a quantum yield of photoluminescence approximately 0,68.

In accordance with the variants of implementation of the present invention created a new luminescent polymeric material based on difibulator complex 1,3,5,7,8-pentamethyl-2,6-diarylpyrimidine (pyrromethene 567). This luminescent polymeric material has a maximum luminescence in the spectral range from 540 to 585 nm when the half-width of luminescence band in the range from 55 to 75 nm, with a quantum yield of photoluminescence in the range from 0.6 to 0.8 and electrical conductivity in the range from 1·10-10up to 5·10-10Ω-1·cm-1. Fluorescent polymeric material according to the present invention can be used to create new light-emitting films. Fluorescent polymeric material based on difibulator complex 1,3,5,1, 8-pentamethyl-2,6-diarylpyrimidine (pyrromethene 567) according to the present invention can be obtained in a new way, i.e. by polymerization in a glow discharge. As a result, the polymer may be precipitated in the form of a thin layer on a substrate.

Proposed in the present invention is advantageous because it provides technological simplicity in implementation. This method is based on the use of commercially available phosphor and does not require solvent to obtain thin layers of semi-conducting luminescent polymer material to create new light-emitting films.

1. The luminous material on the basis of pyrromethene complex, having semi-conducting properties and which is the product of polymerization pyrromethene complex in glow discharge obtained in the form of a polymer layer on a substrate placed between the electrodes or on any of the electrodes.

2. The luminescent material according to claim 1, in which pyrometry the complex is deformity complex 1,3,5,7,8-pentamethyl-2,6-diarylpyrimidine (pyrromethene 567).

3. The luminescent material according to claim 1 or 2, which has a maximum luminescence in the spectral range 540-585 nm at the half-width of the strip 55 to 75 nm and the quantum yield of the photoluminescence of 0.6-0.8.

4. The luminescent material according to claim 1 or 2, which is obtained in the form of a polymer layer with a thickness of 0.01-10 μm.

5. The luminescent material according to claim 1, which has a conductivity of from 1·10-10up to 5·10-10Ω-1cm-1at 20°C.

6. The luminescent material according to claim 1, cat is which is obtained by polymerization in a glow discharge at a temperature of 250-350° C, a residual pressure of 10-1-10-2PA, a discharge power of 0.5-3 watts and time 2-120 minutes

7. The luminescent material according to claim 1, in which the substrate is made of a material selected from the group consisting of metal, dielectric and semiconductor material with a conductive coating.

8. The luminescent material according to claim 1, which is designed to create a film of light-emitting devices.

9. A method of obtaining a fluorescent material according to any one of claims 1 to 8, comprising the polymerization of vapor pyrromethene complex in the glow discharge at low pressure and temperature, providing the necessary vapor pressure, in a period of time sufficient for formation of a polymer layer of the required thickness on a substrate placed between the electrodes or on any of the electrodes.

10. The method according to claim 9, in which as pyrromethene complex use deformity complex 1,3,5,7,8-pentamethyl-2,6-diarylpyrimidine (pyrromethene 567).

11. The method according to claim 9 or 10, in which the polymerization process is carried out in a glow discharge at a temperature of 250-350°C, a residual pressure of 10-1-10-2PA, a discharge power of 0.5-3 watts and within a period of time 2-120 minutes

12. The method according to claim 9, in which the substrate using a substrate made of a material selected from the group consisting of metal, dielectric and semiconductor material with a conductive coating.

13. The method according to claim 9, in which the obtained luminescent material is intended to create a film of light-emitting devices.



 

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SUBSTANCE: invention relates to novel organometallic compounds and to olefin polymerization catalytic systems including such organometallic compounds, and also to a method for polymerization of olefins conduct in presence of said catalytic system. Novel organometallic compound is prepared by bringing into contact (i) compound of general formula I: (I), where Ra, Rb, Rc, and Rd, identical or different, represent hydrocarbon groups; and (ii) Lewis acid of general formula MtR

13
, where Mt represents boron atom and R1, identical or different, are selected from halogen and halogenated C6-C30-aryl groups.

EFFECT: enabled preparation of novel olefin polymerization cocatalysts, which reduce use of excess cocatalyst relative to alkylalumoxanes, do not lead to undesired by-products after activation of metallocene, and form stable catalytic compositions.

14 cl, 1 tbl, 32 ex

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