The method of obtaining poly(2-methoxy-5-(2'-ethylhexyloxy)-1,4 - phenylenevinylene), the electroluminescent device and method of manufacturing

 

(57) Abstract:

Describes how to obtain poly(2-methoxy-5-(2'-ethylhexyloxy)-1,4-phenylenevinylene) (MEH-PPV) for electroluminescent devices, where n corresponds to the values srednekamennogo molecular weight, Mn 17400-40300, mass-average molecular weight Mw 76900-188500 and characteristic viscosity [] 0,46-5,16 DL/g, in which the polymerization reaction of 2-methoxy-5-(2'-ethylhexyloxy)-1,4-bis(chloromethyl)benzene is carried out in polar reaction medium. As the polymerization and the dehydrochlorination polymer precursor is produced by the action of potassium alkoxide, preferably tert-amiloride potassium. The result of the invention to provide a fully soluble linear polymer MEH-PPV with controlled molecular weight and length of polyisoprene, which makes the resulting polymer useful for preparing films (in particular, film electroluminescent devices), as well as the lack of chlorine in the resulting polymer and, as consequence, increase of service life of the polymer), greater efficiency and improving working conditions in the process of synthesis of the polymer. Also described electroluminescent unit (ELU) on the basis of the obtained MEH-PPV. - What the parameters and currents, i.e., high quantum yield, as well as the simplification of the manufacture of the device by reducing the number of stages, decrease the duration of some stages, the possibility of carrying out all operations without creating inert atmosphere. 3 S. and 4 C.p. f-crystals.

The invention relates to methods for organic materials for electroluminescent devices and devices based on them.

A known method of producing polyphenylenevinylene

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as a material for electroluminescent devices, including the application of water-soluble sulfonato polymer - precursor in the form of a coating on a solid substrate with subsequent heat treatment to remove Solonevich groups directly on the substrate, a part of the structure of the electroluminescent device (1-Nature, 1990. V. 347. P. 539). This method is inconvenient in that it requires the additional step of thermal heating of the film together with the substrate, which may cause damage to previously deposited layers (e.g., hole-transport layer). Also known a technique in which the use of the polymer soluble in an organic solvent, for deposition on a substrate by the method of irrigation in the centrifuge. In to the frame main circuit, in particular, poly(2-methoxy-5-(2'-ethylhexyloxy)-1,4-phenylenevinylene) (MEH-PPV) (2-Appl.Phys.Lett. 1991. V. 58. P. 198).

A method of obtaining MEH-PPV

< / BR>
where n corresponds to the mass-average molecular mass Mwpolymer determined by gel permeation chromatography on polystyrene standards, is equal to 300000 (3 - US/5189136). The method involves the polymerization of 2-methoxy-5-(2'-ethylhexyloxy)-1,4-bis(chloromethyl)benzene (I).

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with the formation of the polymer precursor (II)

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and its subsequent dehydrochlorination in a single reactor, and the process is carried out in an environment of tetrahydrofuran (THF) under the action of an excess of base - tert-butoxide potassium.

A method of obtaining MEH-PPV has the following disadvantages.

1. The resulting polymer is only partially soluble in organic solvents (4-US/5679757). Moreover, the polymer solution is unstable at room temperature, that is thixotropic, and when heated gives little soluble gel-like mass (4-US/5679757) that may be associated with the formation of a large number miaocheng links (5-Chem. Mater. 1998. V. 10. P. 3301). As a result of dissolution of the polymer must first leave it for swelling in the R. 1656). This leads to an increase in the duration of the process, as well as the possible uncontrolled changes in the properties of the polymer due to the destruction of its structure by ultrasound.

2. In the synthesis process it is difficult to regulate the molecular weight of the obtained polymer. Even after ultrasonic treatment the resulting solution contains a fraction of the polymer mass in the hundreds of thousands of units and has a high viscosity ([]6 DL/g in THF), making it difficult to obtain coatings by the method of irrigation in the centrifuge and makes impossible the application of some advanced technologies, such as using an inkjet printer for drawing pixels on the active matrix display.

3. In the known method of synthesis used low concentrations of reagents, resulting in a high consumption of solvents. Attempts to increase the concentration of reactants increases the probability of increasing the rate of formation of polymer gel, as well as increase the density of cross-linking of polymer chains. In addition, the solvent used is THF toxic and flammable.

4. Obtained by this method, the derivatives of polyphenylenevinylene contain relatively large (up to 4 wt.%) the amount of chlorine due to lack of money is butoxide potassium into the polymer gel (7-Polymer Bull. 1991. V. 26, N 4. R. 391-394). This can lead to rapid degradation of the electroluminescent device through participation chlorine in the photo - and electrochemical reactions within the layer of polymer and at phase boundaries, for example at the boundary with the metal electrode that injects electrons.

Known electroluminescent unit (ELU) - based polymeric materials consisting of electronic injects a layer of metal, an active luminescent layer of MEH-PPV and an injecting hole of a layer of a mixed oxide of indium and tin (In2ABOUT3-Sn2), which may contain a hole transport layer of conductive polyaniline between a fluorescent and an injecting hole layers (8-Appl.Phys. Letters. 1994. V. 64. N 10. R. 1245-1247). Closest to the present invention, the technical solution is ELU consisting of electronic injects a layer of aluminum-lithium alloy, an active luminescent layer of MEH-PPV, the hole transport layer based on conducting polyaniline and an injecting hole of a layer of a mixed oxide of indium and tin In2O3-SnO2(9-J. Appl.Phys. 1995. V. 77. N 2. R. 694-698).

The disadvantages of the known device should be attributed to the relatively low quantum yield.

A known method of manufacturing described above ELU (9-J. Appl.Phys. 1995. V. 77. N 2. R. 694-698), comprising the following sequence of operations.

1) Drawing on hole injects a layer of a mixed oxide of indium and tin (In2ABOUT3-Sn2), hole transport layer consisting of conductive polyaniline with the addition of polyester resin. This operation is carried out by watering in the centrifuge m-krasilnogo solution containing a complex of polyaniline with camphorsulfonate (CSC) and additive polyester resin, followed by drying for 12 hours at 50 C.

2) Application of active luminescent layer MEH-PPV by centrifuging from a solution in xylene.

3) Deposition in high vacuum (210-7mm RT.CT.) aluminum-lithium alloy containing Li 0,2%.

The known method is complex technology and high labour costs due to the following circumstances.

1. The process of applying MEH-PPV includes additional stages of swelling of the polymer in the solvent and processing of ultrasound gel, necessary for dissolution of the polymer.

2. The complex of polyaniline and the stewards prepare long-term mechanical mixing these componentkey stages of preparation of a solution of polyester resin and mixing this solution with a solution polyanilines salt.

4. Used to prepare films of polyaniline solvent - m-cresol requires a long drying time (12 hours) and poor working conditions because it is a toxic reagent.

5. The need for all stages of the preparation of polyaniline film in an inert atmosphere.

The aim of the present invention is to provide materials for ELU, free from the above shortcomings, as well as the creation ELU with improved performance and simplify its manufacturing technology.

The problem is solved in that in the method of obtaining MEH-PPV reaction polymerization of the monomer I is carried out in a polar reaction medium (aromatic hydrocarbons: benzene, toluene, ethylbenzene, isopropylbenzene, n-propylbenzene, tert-butylbenzoyl, n-butylbenzoyl, 1,3,5-trimethylbenzene (mesothelin), 1,2,3,4-tetrahydronaphthalen (tetralin), 1-methylnaphthalene, o -, m - or p-xylene, preferably toluene or toluene with a small controlled addition of tert-amyl alcohol), and the basis is soluble in slightly polar environment the potassium alkoxide, preferably tert-amyloxy potassium. In addition, it uses a higher concentration of initial reagents and, consequently, lower the standing of electronic injects a layer based on aluminum alloy, active luminescent layer of MEH-PPV, the hole transport layer of conductive polyaniline and an injecting hole of a layer of a mixed oxide of indium and tin (In2O3-SnO3), as the active luminescent layer is used MEH-PPV, obtained as indicated above, and as a hole transport layer using doped carboxylic acids (QC) or n-toluensulfonate (PTSC) polyaniline, which can be plasticized polyvinyl alcohol (PVA).

The result of the invention to provide a fully soluble linear polymer MEH-PPV with controlled molecular weight and length of polyisoprene. Characteristic viscosity solutions of the obtained polymers in a controlled way varies in the range []=0,46-5,16 DL/g, whereas for the polymer obtained in a known manner, [] even after ultrasonic treatment more than 5 DL/g Polymers with low viscosity are completely dissolved in the toluene and o-xylene, more high molecular weight polymers are poorly soluble in aromatic hydrocarbons, but completely soluble in chloroform, THF, tetrachloroethane, chlorobenzene, and the resulting solutions are stable at room temperature, and DL devices (6-J. Appl.Phys. 1994. V. 76. R. 1656), does not require the use of ultrasound. These properties make the polymer more convenient for the preparation of films, in particular films in ELU than the polymer obtained in a known manner. In addition, the invention is higher efficiency, reduced fire hazards and improving working conditions. The result of the invention is the absence of chlorine in the resulting polymer, which increases the service life of the polymer.

This result is achieved in that in the method of obtaining MEH-PPV reaction polymerization of the monomer I is carried out under milder conditions compared with the known method, which uses a polar reaction medium (aromatic hydrocarbons: benzene, toluene, ethylbenzene, isopropylbenzene, n-propylbenzene, tert-butylbenzoyl, n-butylbenzoyl, 1,3,5-trimethylbenzene (mesothelin), 1,2,3,4-tetrahydronaphthalen (tetralin), 1-methylnaphthalene, o-, m - or p-xylene, preferably toluene or toluene with a small controlled addition of tert-amyl alcohol), and the basis is soluble in slightly polar environment the potassium alkoxide, preferably tert-amyloxy potassium. Milder conditions of the synthesis privilege predecessor (II), which leads to the improvement of the solubility of the polymer and the complete removal of chlorine from the final product. When conducting the reaction in the environment of aromatic hydrocarbon is obtained a polymer with a lower molecular weight than the conventional method of synthesis. The addition of small amounts (up to 5 vol.%) tert-amyl alcohol to the solution of the original monomer in aromatic hydrocarbons produces a significant increase in the molecular weight of the obtained polymer, and controlled change of the alcohol concentration in the initial reaction mixture allows you to get completely soluble in these solvents are linear polymers of desired molecular weight and a specified length of chain polyisoprene. In addition, this result is achieved by using much higher concentration of initial reagents in comparison with the known method, which allows to reduce the consumption of solvent and precipitant and solvent used is toluene is cheaper, less flammable and less toxic compared to the THF used in the prototype. This leads to greater efficiency of the process, to reduce fire hazard and improve working conditions.

Technical resole high brightness at lower voltages and currents, that is, high quantum yield, as well as the simplification of the manufacture of the device by reducing the number of stages, decrease the duration of some stages, the possibility of carrying out all operations without creating inert atmosphere.

This technical result is achieved by the electroluminescent device consisting of electronic injects a layer based on aluminum alloy, an active luminescent layer of MEH-PPV, the hole transport layer of conductive polyaniline and an injecting hole of a layer of a mixed oxide of indium and tin (In2O3-SnO2), as the active luminescent layer is used soluble MEH-PPV, obtained as indicated above, and as a hole transport layer using doped carboxylic acids (QC) or n-toluensulfonate (PTSC) polyaniline, which can be plasticized polyvinyl alcohol (PVA), which provides a high flexibility of the coating and warrants through defects. The latter leads to the reduction of the leakage current and increase the overall quantum yield. This technical result is also achieved by the fact that in the method of manufacturing the second layer of a mixed oxide of indium and tin layers are p-doped polyaniline, active luminescent layer of MEH-PPV and electronic injects a layer of aluminum alloy, for applying a layer MEH-PPV used soluble MEH-PPV, obtained by the above method, and for applying a layer of p-doped polyaniline use a solution containing the following components (mass%): polyaniline 0.6 to 1.5; PTSC or QC 0.06 to 0.5; the polyvinyl alcohol 0-1,5; formic acid - the rest. The use of a mixture of polyaniline and PTSC or QC in formic acid with the addition of PVA allows drying at room temperature for a few minutes and ensures continuity of coverage.

The invention is illustrated by the following examples.

Example 1. The reproduction known way for MEH-PPV [4].

to 1.00 g (3 mmol) of monomer I was dissolved in 20 ml of anhydrous THF. To the resulting solution was added dropwise a solution 2,12 g (18 mmol) of tertbutoxide potassium in 80 ml of anhydrous THF. Gelation was observed after the addition has taken 1/3 of the solution. The reaction mixture was stirred at room temperature for 24 hours and then poured into 500 ml of methanol. Received a red precipitate was washed with distilled water, dried in vacuum at 50oC, Rast is methanol and dried in vacuum at 50oC. the polymer Yield 0.35 g (45%). The chlorine content according to the elemental analysis of 1.1%. The characteristic viscosity solution in THF []=5,90 DL/g Characteristics of the molecular weight distribution determined by GPC method according to polystyrene standards: srednekislye molecular weight MP=49600, mass-average molecular weight Mw=165000, the polydispersity Mw/Mn=3,33. The maximum absorption (solution in THF) 503 nm. IR bands (tablet CVG): 703, 727, 770, 855, 963, 1035, 1255, 1350, 1410, 1460, 1500, 2860, 2925, 2960, 3057 cm-1that is close to the prototype [4]. The maximum photoluminescence (exciting line 436 nm): solution in THF - 560 nm, 600 nm (shoulder); film - 595 nm, 630 nm (shoulder). Quantum yield of photoluminescence for a solution in o-xylene of 0.64. For the preparation of polymer solutions are required stage of swelling and ultrasonic treatment.

Example 2. Synthesis of soluble MEH-PPV.

to 1.00 g (3 mmol) of monomer I, was dissolved with stirring in 14.7 ml of toluene. To the resulting solution for 10 min was added dropwise 1,967 g (18,02 mmol) tert-amiloride potassium in 15 ml of toluene. The reaction mixture was stirred pikantnoi temperature for 24 hours and was poured with stirring into 200 ml of methanol. The precipitate was washed with 50 ml of methanol, distilled water, chlorine 0,0%. []= 0,46 DL/g IR-bands (film) 740, 770, 810, 860, 965, 1037, 1200, 1250, 1350, 1410, 1460, 1500 cm-1.

Example 3. Synthesis of soluble MEH-PPV.

Analogously to example 2, but the monomer I was dissolved in a mixture of toluene and tert-amyl alcohol, taken in the ratio of 100:1,35. The polymer yield 0,281 g (36%). The chlorine content of 0.0%. []=to 0.80 DL/g, MT=17400, Mw=76900, Mw/Mn=4,42. The maximum absorption (solution in chloroform) 489 nm. The maximum photoluminescence (exciting line 436 nm): a solution of chloroform - 560 nm, 600 nm (shoulder); film - 600 nm, 640 nm (shoulder). Quantum yield of photoluminescence for a solution in chloroform of 0.59.

Example 4. Synthesis of soluble MEH-PPV.

Analogously to example 2, but the monomer I was dissolved in a mixture of toluene and tert-amyl alcohol, taken in the ratio of 100:4,06. The polymer yield 0,328 g (42%). The chlorine content of 0.0%. []= 2,73 DL/g, MT=34100, Mw=127000, Mw/Mn=to 3.73. The maximum absorption (solution in chloroform) 489 nm. The maximum photoluminescence (exciting line 436 nm, a solution in chloroform) - 560 nm, 600 nm (shoulder).

Example 5. Synthesis of soluble MEH-PPV.

Analogously to example 2, but the monomer I was dissolved in a mixture of toluene and tert-amyl alcohol, taken in the ratio of 100: 6,27. The polymer yield 0,343 g (44%). The chlorine content of 0.0%. ]=5,16 DL/g, Mn=40300, Mw=188500, Mw/Mn= 4,68. A maximum of pogles the . The maximum photoluminescence (exciting line 436 nm): a solution of chloroform - 560 nm, 600 nm (shoulder), film - 600 nm, 640 nm (shoulder).

Example 6. The electroluminescent device.

Use a glass substrate with a transparent layer of a mixed oxide of indium and tin with resistance 30-70 Ω/square, which by centrifuging put a layer of polyaniline with PTSC thickness of 0.05-0.1 μm from a solution in formic acid at the following content, wt.%: polyaniline 0.6 to 1.5; PTSC 0.06 to 0.5; the formic acid - the rest. The applied layer is dried at a temperature of 60-70oC for 30 min and Then centrifuging cause the active layer is soluble MEH-PPV thickness of 0.08 to 0.1 ám of orthoxylene solution (8 mg/ml, vaskos [] about 5 DL/g) and dried for 15-20 min at 60-70oC. the Sample is placed in a vacuum installation VUP-4, pump out in a dynamic mode to vacuum 10-6mm RT.art., heated in vacuum to 100oC for 2 hours, and after cooling to room temperature, sprayed metal electrode by evaporation of aluminum-lithium alloy. The thickness of the metal electrode is about 0.1 μm. The area of the illuminated surface of 4-5 mm2. Received ELU has trace the current of 0.025 mA;

- brightness when 3 V is 660 CD/m2that is 60% higher than for the prototype (400 CD/m2);

- brightness 1200 CD/m2is achieved at a voltage of 3.4 V and a current of 2 mA, the luminance of 4000 CD/m2;

when the voltage of about 5 V, which is twice lower than for the prototype (10) and a current of about 8 mA.

Example 7. The electroluminescent device.

ELU, prepared as in example 6, but when applying a layer of polyaniline with PTS in solution add PVA in an amount of 0.6 to 1.5 wt.%. For this ELU threshold of occurrence of radiation slightly increased compared to example 1 (1.7 V and 0.03 mA), but the quantum efficiency (photons per electron) is about 1.5 times higher: brightness 1200 CD/m2is achieved at a current of 1.7 mA.

Sources of information

1. J. H. Buroughes et al. Nature v.347, p.539 (1990).

2. D. Brawn, A. J. Heeger, Appl.Phys.Lett. v.58, p.198 (1991).

3. F. Wudl, G. Srdanov, US Pat. 5189136 (1993).

4. F. Wudl, S. Hoger, US Pat. 5679757 (1997).

5. Y. Liu et al. Chem. Mater. v.10, p.3301 (1998).

6. I. D. Parker, J. Appl. Phys. v.76, p. 1656 (1994).

7. Bing R. Hfieh, Polymer Bull. (1991) v.26, N 4, p.391-394.

8. Y. Yang, A. J. Heeger, Appl. Phys.Letters (1994) v.64, No. 10, p. 1245-1247.

9. Y. Yang, E. Westerweele, C. Zhang, P. Smith, A. J. Heeger, J. Appl. Phys. (1995) v.77, No. 2, p.694-698.

1. The method of obtaining poly(2-methoxy-5-(2'-ethylhexyloxy 17400-40300, the mass-average molecular weight Mw 76900-188500 and characteristic viscosity [] 0,46-5,16 DL/g,

including the polymerization of 2-methoxy-5-(2'-ethylhexyloxy)-1,4-bis(chloromethyl)benzene, followed by dehydrochlorination of the formed polymer precursor by the action of potassium alkoxide in an organic solvent, characterized in that the polymerization of lead in the environment of polar aromatic hydrocarbon.

2. The method according to p. 1, characterized in that the polymerization of lead in the environment toluene.

3. The method according to p. 1, characterized in that as alkoxide use potassium tert-amyloxy potassium.

4. The method according to p. 2, characterized in that the aromatic hydrocarbon is injected controlled additive tert-amyl alcohol.

5. The electroluminescent device consisting of electronic an injecting layer (cathode) made of aluminum alloy, an active luminescent layer of poly(2-methoxy-5-(2'-ethylhexyloxy)-1,4-phenylenevinylene), hole transport layer based on the p-doped polyaniline and an injecting hole layer (anode) of a mixed oxide of indium and tin In2ABOUT3-Sn2, characterized in that as the active luminescent layer it setnogo layer is used polyaniline, doped carboxylic acids or n-toluensulfonate, which can be plasticized polyvinyl alcohol.

6. The electroluminescent device according to p. 5, characterized in that the doped polyaniline plasticized polyvinyl alcohol.

7. A method of manufacturing an electroluminescent device by successively applying onto a glass substrate coated with a layer of a mixed oxide of indium and tin layers are p-doped polyaniline, and electronic injects a layer of aluminum alloy, characterized in that as the active luminescent layer using poly(2-methoxy-5-(2'-ethylhexyloxy)-1,4-phenylenevinylene) obtained under item 1, and for applying a layer of p-doped polyaniline use a solution containing the following components, wt. %: polyaniline 0.6 to 1.5; polyvinyl alcohol 0-1,5; n-toluensulfonate or carboxylic acid 0.06 to 0.5; the formic acid rest.

 

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2 cl, 3 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to polymer material engineering, particularly to modification of porous materials by forming coatings. Modified porous polymer material can be used to make components for use in different scientific and engineering fields, for example wicks for raising hydrocarbon liquids through a capillary effect, filter elements, carrier matrix for active low-molecular components as part of structures bearing a power load, for example, wings of a light aeroplane. The disclosed method includes forming, on the surface of structural elements of a matrix of the initial porous material, a continuous coating from a polymer with physical and mechanical properties different from that of the polymer of the matrix of the initial porous material. The coating is formed as a result of synthesis of a heat-resistant polymer - poly-para-xylylene via gas-phase polymerisation on the surface. Synthesis of a film of poly-para-xylylene is carried out at temperature of the walls of the polymerisation chamber of 20-25°C and pressure of the gaseous monomer (para-xylylene) of about 5-8 Pa, wherein directed movement of monomer molecules through the matrix of the initial porous material is facilitated in the chamber. Also declared is a composite porous material containing a matrix with through porosity and a continuous coating of poly-para-xylylene with thickness of 0.2-0.3 mm on the surface of structural matrix elements. The technical result is increasing heat resistance of the modified porous plastic 2-3-fold to 250-300°C (Vicat softening point); uniaxial compression strength of the modified material is significantly greater than that of the initial material ( 2 times greater); resistance of the modified porous plastic to solvents increases since the modifying coating dissolves at high temperature only in very strong solvents.

EFFECT: method significantly supplements the range of porous materials for various purposes.

2 cl, 3 dwg

FIELD: organic synthesis.

SUBSTANCE: invention provides novel compound: 1-[2-(4,6-dichloro-[1,3,5]triazine-2-ylamino)phenyl]-benzo[d][1,3]oxazine-4-one, characterized by yellow luminescence. Preparation of this compound comprises preliminarily preparing 2-(2-aminophenyl)-benzo[d][1,3]oxazine-4-one by reaction of anthralic acid with thionyl chloride followed by reaction of thus prepared compound with cyanuric acid chloride. Compound is characterized by fluorescence maximum at 560 nm and spare solubility in most organic solvents. The latter enables use of the compound in polygraphic inks as fluorescent pigment.

EFFECT: enlarged assortment of luminophors.

2 cl, 1 dwg

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