Moo2 powder, methods of manufacturing plate from moo2 powder (their versions), element and method of manufacturing thin film from it, method of sputtering with application of said plate

FIELD: chemistry.

SUBSTANCE: invention can be used in manufacturing organic light-emitting diodes, liquid-crystal displays, plasma display panel, thin-film solar cell and other electronic and semi-conductor devices. Claimed is element, including target of ionic dispersion, where said target includes processed MoO2 plate of high purity. Method of such plate manufacturing includes isostatic pressing of component consisting of more than 99% of stoichiometric MoO2 powder into workpiece, sintering of said workpiece under conditions of supporting more than 99% of MoO2 stoichiometry and formation of plate which includes more than 99% of stoichiometric MoO2. In other version of said plate manufacturing component, consisting of powder, which contains more than 99% of stoichiometric MoO2, is processed under conditions of hot pressing with formation of plate. Method of thin film manufacturing includes stages of sputtering of plate, which contains more than 99% of stoichiometric MoO2, removal of MoO2 molecules from plate and application of MoO2 molecules on substrate. Also claimed is MoO2 powder and method of said plate sputtering with application of magnetron sputtering, pulse laser sputtering, ionic-beam sputtering, triode sputtering and their combination.

EFFECT: invention allows to increase work of output of electron of ionic sputtering target material in organic light-emitting diodes.

16 cl, 5 ex

 

The present invention relates to a powder of Moo2the method of manufacturing a plate of powder MoO2(options), element and method of manufacturing a thin film thereof, and to a method of sputtering with the use of said plate.

The indium oxide and tin (PSI), doped zinc PSI and doped aluminum ZnO represent typical materials of the target ion sputtering. However, when they are used in applications such as, for example, in the organic light-emitting diodes, their work output (typically about 4.7 eV) does not match well the desired light-emitting operation of the output.

Thus, the objective of the proposed invention is to provide a material of the target ion sputtering, which could be used for the manufacture of organic light-emitting diodes that do not have problems and limitations of the materials of the target ion sputtering of PSI and doped zinc PSI.

The solution to this problem is the powder MoO2containing more than 99% of the stoichiometric amount MoO2.

This powder MoO2high purity obtained by reduction of ammonium molybdate or molybdenum trioxide with hydrogen as a reducing agent in a rotary kiln or furnace boat (boat furnace). Compaction of the powder by press the Finance/sintering, hot pressing and/or hot isostatic pressing is used for the production of discs, plates or plates, which are used as ion sputtering targets. The form of a disk, tiles or plates MoO2sprayed on the substrate, using a suitable method, sputtering or other physical means to obtain a thin film having a desired film thickness. These thin films have properties, such as electrical, optical properties, properties, surface roughness and homogeneity, which are comparable or superior to those of indium oxide and tin (PSI), doped zinc PSI and doped aluminum ZnO in terms of transparency, conductivity, work function, homogeneity and surface roughness. These thin films can be used in organic light emitting diodes (acid), liquid crystal display (LCD), plasma display panel (PDP)display autoelectronic emission (AED), thin-film solar cell, ohmic contacts with low resistance and other electronic and semiconductor devices.

Non-operating examples, or otherwise indicated, all numbers or expressions that refer to quantities of ingredients, reaction conditions, etc. used in the specification and the claims the invention, understood as modified in all instances by the term "about". Various numerical intervals disclosed in this patent application. Since these intervals are continuous, they include every value between the minimum and maximum values. Unless explicitly stated otherwise, different numerical intervals indicated in this application are approximations.

Used herein, the term "MoO2high purity" refers to materials and compounds that contain more than 99.95 percent by weight of Moo2and at least 99% by weight of the phase of Moo2.

Used herein, the term "stoichiometric powder of Moo2" refers to the powder, which contains the specified percentage of MoO2then there is Mo and About in the ratio of 1:2. As a non-limiting example 99%stoichiometric powder MoO2would contain 99% powder MoO2and 1% of other material, with a non-limiting example thereof is a Moo3.

The present invention is to produce a powder MoO2high purity recovery of ammonium molybdate or molybdenum trioxide with hydrogen as the reducing agent as a reducing agent in a rotary kiln or furnace boat. Compaction of the powder by pressing/sintering, hot pressing and/or hot isostatic what about pressing use, to make the disks, tiles or plates, which are used as targets ion sputtering. The form of a disk, tiles or plates MoO2sprayed on the substrate, using a suitable method, sputtering or other physical means to provide a thin film having a desired film thickness. These thin films have properties, such as electrical, optical properties, properties, surface roughness and homogeneity, which are comparable or superior to those of indium oxide and tin (PSI), doped zinc PSI and doped aluminum ZnO in terms of transparency, conductivity, work function, homogeneity and surface roughness. These thin films can be used in organic light-emitting diodes and other electronic and semiconductor devices.

Used herein, the term "work function" refers to the energy required to move an electron in the atom from the Fermi level to the vacuum level, i.e. outside of the atom. In the present invention, the output operation will vary depending on surface conditions, such as impurities.

Used herein, the term "organic light-emitting diode" refers to an electronic device made by placing a series of organic thin films between two conductors is. When application of the electric current emitted a bright light, usually by electrophosphorescence.

Variant implementation of the present invention is directed to a method of producing powder MoO2high purity. This method includes:

(a) placing a molybdenum component in an oven and

(b) heating the molybdenum component in a furnace containing a reductive atmosphere.

During implementation of the invention can be used with any suitable source of molybdenum as molybdenum component. Suitable sources of molybdenum include compounds that can provide high purity MoO2when used in this way. Suitable sources for molybdenum component include, but are not limited to, salt dimolybdate ammonium, molybdenum trioxide, and combinations thereof.

When carrying out the invention the molybdenum component is heated to a sufficiently high temperature to convert the molybdenum component in MoO2high purity, typically more than 99% of the stoichiometric powder MoO2. The temperature in the furnace in this way can be less than 1250°C., in some cases less than 1000°C., in other cases less than 800°C, in some situations less than 700°C., and in other situations less than 650°C. Also, the temperature in the furnace in the present method may be at least 100°C, is some cases at least 250°C, and in other cases at least 500°C. the temperature in the furnace can be any of these temperatures, or it can be located between any of the values of the temperatures in the furnace, above.

In the embodiment of the invention the molybdenum component is heated at a temperature furnace for a period of time sufficient to convert the molybdenum component in MoO2high purity, typically more than 99% of the stoichiometric powder MoO2. This time period may vary depending on the temperature in the furnace, where higher temperatures usually result in shorter required time of heating. The heating time may be at least 5 minutes, in some cases at least 10 minutes, in other cases at least 15 minutes, in some situations at least 30 minutes, in other situations at least 45 minutes, in some circumstances at least one hour, and in other circumstances at least 90 minutes. Also, the heating time can be up to 8 hours, in some cases up to 6 hours, in other cases up to 5 hours, in some situations up to 4 hours, and in other situations up to 3 hours. The period of time when the molybdenum component is heated at a temperature in the furnace can be any of the above time periods, or it can be placed between any of the time periods specified what's above.

Any suitable furnace may be used in the present invention. Suitable furnaces include those that can expose the molybdenum component to effect the desired temperature for the desired time periods specified above, and if desired the surrounding environments and/or atmospheres. Suitable furnace, which can be used in the present invention include, but are not limited to, a stationary tubular furnaces, rotary tube furnaces and kilns.

Any suitable atmosphere may be used in the oven of the present invention. The appropriate atmosphere support the formation of Moo2high purity, typically more than 99% of the stoichiometric powder MoO2. In the embodiment of the present invention in a furnace using regenerative atmosphere. In a specific embodiment of the present invention, the reducing atmosphere comprises hydrogen. In the embodiment of the present invention the molybdenum component is placed in a flat-bottomed boat, which is placed in a furnace and heated in a desirable atmosphere, as described above. In a specific embodiment of the invention 6,8 kg dimolybdate ammonium placed in a flat-bottomed boat and the boat is heated in a stationary tubular furnace for two to three hours when temperature is round from 500°C to 700°C.

Powder MoO2can be characterized as having an average particle size of at least 0.1 micron, in some cases at least 0.5 micron, and in other cases at least 1 μm. Also powder MoO2may have an average particle size of 50 microns, in some cases up to 100 μm. The average particle size of the powder MoO2can be any value or can range between any of the values specified above.

Another object of the invention is a method of manufacturing a plate, which includes:

(A) isostatic pressing component of more than 99% of the stoichiometric powder MoO2in the workpiece;

(B) sintering in vacuum and/or pressure of the workpiece in the conditions to support more than 99% of the stoichiometry of Moo2; and

(B) forming plate, which includes more than 99% of the stoichiometric NGO2.

A further object of the invention is a method of manufacturing a plate consisting of a powder containing more than 99% of the stoichiometric MoO2process in the conditions of hot pressing, thereby forming a plate, which includes more than 99% of the stoichiometric NGO2.

Conditions of hot pressing usually means high pressure, such that the plate is formed with a low speed relative deformation at a temperature sufficient is high, to stimulate the process of sintering and deformation process. For MoO2this usually requires 1000°C to achieve the desired density. In one embodiment of the invention, where the plate is made in the conditions of hot pressing stage hot pressing is carried out with a transition in the liquid phase, contributing to hot pressing, and the method of pressing includes the compaction of the powder at the temperature when the liquid and solid phases coexist due to chemical reactions, partial melting or formation of eutectic liquid.

Another object of the invention is the element that includes the ion sputtering target, where the target ion sputtering includes machined plate of MoO2high purity. The ion sputtering target is made by processing wafers, comprising more than 99% of the stoichiometric NGO2up until not receive the target ion sputtering with desirable properties and/or dimensions. Processing, which expose the plate may include any processing that is suitable for the manufacture of ion sputtering targets having suitable properties/dimensions. Examples of suitable processing stages include, but are not limited to, laser cutting, milling, handling and processing on a lathe. The target ion sputtering m which may be polished, to improve the roughness of its surface. Examples of suitable diameters for circular targets ion sputtering, for example, can range from 1 inch (2.54 cm) to 25 inches (63.5 cm), preferably from four inches (10.2 cm) to eight inches (20.4 cm). Examples of suitable thicknesses for such annular ion sputtering targets can be in the range from 0.15 cm to 20 cm, preferably less than one inch (less than 2.54 cm).

Can be applied to any suitable pressure to form individual blanks, when the powder of Moo2is subjected to isostatic pressing. Suitable pressures are those which allow the pressing metal powder between the powder MoO2and the workpiece. The pressure can be at least of 34.5 MPa (5000 psi), in some cases at least of 51.7 MPa (7500 psi), in other cases at least 68,9 MPa (10000 psi), in some situations at least 103,4 MPa (15000 psi) and in other situations at least 137,9 MPa (20000 psi). Also the pressure can be up to 689,47 MPa (100,000 pounds per square inch), in some cases up to 517,1 (75000 pounds per square inch), in other cases up to 344,7 MPa (50000 pounds per square inch), in some situations up to 275,8 MPa (40000 pounds on kV is druty inch), and in other situations up to 206,8 MPa (30000 psi). The pressure at the stage isostatic pressing can be any of the above pressure values or can be located between any of the values specified above.

Suitable sintering conditions are those in which the powder MoO2generates coherent coherent mass without melting. The length of time of sintering will depend on the sintering temperature. In the embodiment of the invention the workpiece is sintered in vacuum or in a suitable partial pressure of oxygen for at least 15 minutes, in some cases at least 30 minutes, in other cases at least 1 hour, in some situations at least 2 hours, and in other situations at least 3 hours. Harvesting can be sintered in vacuum in a period of time up to 10 hours, in some cases up to 20 hours, in other cases up to 7 hours, in some situations up to 6 hours, and in other situations up to 5 hours. The period of time for which the workpiece is sintered in vacuum or in a suitable partial pressure of oxygen, may be any of the specified periods of time or may be placed between any of the time periods specified above.

The sintering temperature is at least 1000°C, in some cases at least 1100°C, in other cases, p is at least 1200°C, and in some situations at least 1250°C. Also, the sintering temperature can be up to 2500°C, in some cases up to 2000°C, in some situations up to 1750°C, and in other situations up to 1500°C, depending on the exact composition of the powder MoO2and the workpiece. The sintering temperature may be any temperature or can be located between any of the temperature values specified above.

Any suitable conditions of pressing can be used in the present invention. Suitable conditions of extrusion are those in which the pressed and sintered powder of Moo2can be formed in the plate while maintaining the stoichiometry of more than 99% of Moo2.

In the embodiment of the invention the plate is subjected to hot isostatic pressing.

Plate, formed by the proposed method has a density that is at least 85%, in some cases at least 90%, in other cases at least 95%, and may be up to 99%, and in some cases up to 100% of theoretical density MoO2. The density of the plate can be any of the values specified density or can be placed between any of the values of density specified above.

The object of the invention is also a method of atomization, which includes Pomerania plate, including b is over 99% stoichiometric MoO 2described above, the sputtering conditions and thus the spray plate.

Any suitable method of atomization can be used in the invention. Suitable methods are those that are able to precipitate a thin film on the wafer. Examples of suitable methods include spraying, but are not limited to, magnetron sputtering, pulsed laser sputtering, ion beam sputtering, triode sputtering, and combinations thereof.

In addition to sputtering, the deposition of a thin film on the wafer can be accomplished in other ways. Suitable methods of thin film deposition on the wafer include, but are not limited to, electron-beam deposition and physical means, such as physical vapor deposition.

The present invention also is directed to a method of manufacturing a thin film. The method includes the stage of spraying plate, comprising more than 99% of the stoichiometric MoO2, remove molecules of Moo2with plates and deposition of molecules of Moo2on the substrate, to thereby form a thin film.

Suitable methods of atomization, which are described above, can be used in this embodiment of the invention.

Thin film deposited by the present method may be of any desirable thickness. The film thickness may be the least about 0.5 nm, in some situations, 1 nm, in some cases at least 5 nm, in other cases at least 10 nm, in some situations at least 25 nm, in other situations at least 50 nm, in some circumstances at least 75 nm, and in other circumstances at least 100 nm. Also, the film thickness can be up to 10 μm, in some cases up to 5 μm, in other cases up to 2 microns, in some situations up to 1 μm, and in other situations up to 0.5 μm. The film thickness can be any value or can range between any of the specified values.

Thin film obtained in accordance with the invention, as described above, has a work function that is higher than the work function of the films of indium oxide and tin, having the same dimensions. Also, the output operation can be from 5.0 eV to 6.0 eV, and in some cases at least 5.2 eV, or any of these values individually.

Thin film has a surface roughness that is less than the surface roughness in comparison with a thin film of indium oxide and tin. In particular, the surface roughness can be less than 10 nm, in some cases, less than 5 nm, in other cases less than 4 nm, and in some situations less than 3 nm. The surface roughness is usually more than 0.1 nm. The surface roughness of the mo is et to be any value or can range between any of the values above.

Thin film has an average transmittance of 85% at a wavelength of from 350 to 800 nm.

In an additional embodiment of the invention a thin film has a resistivity that is less than 500 µohm×cm, in some cases less than 300 µohm×cm, and in other cases less than 250 µohm×see Specific resistance of a thin film is usually more than 1 µohm×see Specific resistance of a thin film can be any value or can range between any of the values specified above. It is a high conductivity metal behavior as a function of temperature.

Possible and obtain a very thin film. However, she has a thickness of at least 100 Å, in some cases at least 250 Å, and in other cases at least 500 Å. In this embodiment of the invention, a thin film may have a thickness of 5000 Å, in some cases up to 3000 Å, in other cases up to 2500 Å, and in some situations up to 2000 Å.

The invention can be used to produce organic light-emitting diode, which includes:

(a) a metal electrode;

(b) electron transport layer;

(C) an emitter layer;

(g) electrically conductive polymer (hole transport layer); and

(d) a thin film described above, located on substra the E.

Any suitable substrate can be used in the invention. Suitable substrates for thin films used in organic light-emitting diode, include, but are not limited to, plastic substrates, glass substrates, ceramic substrates, and combinations thereof. The plastic substrates include, but are not limited to, polynorbornene, polyimide, polyarylate, polycarbonate, polietilentereftalat (PAN), polyethylene terephthalate (PET) and the like. A non-limiting example of the ceramic substrate includes sapphire.

The invention covers products used in various applications. In one embodiment of the invention a thin film made in accordance with the invention can be used in applications in thin film transistors (TFT), liquid crystal displays (LCD). In another embodiment, the invention comprises a thin film used in solar cells and batteries. In one embodiment, the invention is a containing LCD device that has both (1) the common electrode (about 1500), and (2) a pixel electrode (about 500). In applications in thin film solar cells the invention covers the solar cells, in which the Moo2functions as a front electrode for Shadowmaster illustrative device: front contact of MoO 2/layer with hole conductivity/layer p-n junction/layer with electron conductivity/back contact of Al, in which the layer with hole conductivity releases electrons when it is subjected to the action of light, which leads to the lack of electrons, and the layer with electron conductivity is charged negatively. In another embodiment, the invention encompasses ohmic contacts (transparent contacts the oxide/metal), so that lowering the total contact resistance, and to allow light emission from light emitting diodes (such as GaN LED)or diode lasers.

Films according to the invention, containing more than 99% of the stoichiometric NGO2posted on at least part of the substrate, can be used for optical display devices. In this embodiment of the invention optical display devices include a film that contains more than 99% of the stoichiometric MoO2posted on at least part of the substrate.

The film according to the invention can be formed by:

(a) spraying plate, comprising more than 99% of the stoichiometric MoO2;

(b) removing molecules MoO2with plates;

(C) applying molecules MoO2on the substrate, thereby forming a thin film MoO2.

The film can be obtained by:

(a) spraying the plates include what it is more than 99% of Mo;

(b) removing molecules Mo with plate;

(C) forming molecules MoO2at a partial pressure of oxygen in the chamber to obtain a thin film MoO2on the substrate.

Any suitable method of spraying can be used. Suitable methods of atomization, which can be used include, but are not limited to, magnetron sputtering, pulsed laser sputtering, ion beam sputtering, triode sputtering, and combinations thereof. Thin film has a thickness of at least 0.1 nm, in some cases at least 0.5 nm, in other cases at least 1 nm, in some situations at least 2 nm, in other situations at least 5 nm, in some examples at least 8 nm, in other examples, at least 10 nm, and in specific situations at least 25 nm. Also, the film may have a thickness up to 10 μm, in some cases up to 7.5 μm, in other cases up to 5 microns, in some situations up to 2.5 microns, in other situations up to 1 μm, in some instances up to 0.5 μm, in other examples to 0.25 μm, and in the specific examples to 0.1 μm. The film thickness can be or can range between any of the values specified above.

Thin film used in the optical display device may have a film thickness from 50 Å to 2500 Å.

The optical device can include one and the and more suitable films containing MoO2. He limiting examples of suitable films include, but are not limited to, films of a single phase MoO2doped with impurities film MoO2doped tin oxide film MoO2doped tin oxide and indium films MoO2doped ZnO/In2O3film MoO2doped ZnO/SnO2/In2O3film MoO2doped ZnO films MoO2doped SnO2film MoO2doped ZnO/Al2O3film MoO2doped Ga/ZnO films MoO2doped GaO/ZnO films MoO2doped stannate zinc (Zn2SnO4) film MoO2and the composite film MoO2-Moo3.

Spray the plate can be any suitable shape and size. As a non-limiting example, a spray plate may be in the shape of a square, rectangle, circle or oval. In a specific embodiment of the invention a square spray plate may be square and have dimensions of 0.1 cm × 0.1 cm to 5 cm × 5 cm, in some cases, from 0.5 cm × 0.5 cm to 4 cm × 4 cm, in other cases from 1 cm × 1 cm to 3 cm × 3 cm, in some situations, from 2 cm × 2 cm to 3 cm × 3 cm, and in other situations square spray plate has dimensions of about 2.5 cm to about 2.5, see

In the case of the rectangular shape of raspily the may plate may have a shorter side length of at least 0.1 cm, in some cases at least 0.5 cm, in other cases at least 1 cm, in some situations at least 2 cm, in other situations at least 2.5 cm, in some examples at least 3 cm, in other examples, at least 4 cm, and in specific situations at least 5 see Also the longer side of the rectangle can be up to 6 cm, in some cases up to 5 cm, in other cases up to 4 cm, in some situations up to 3 cm, in other situations up to 2.5 cm, in some instances up to 2 cm, in other instances up to 1 cm, and in the specific examples to 0.75, see the dimensions of the rectangular spray plate can vary between any of these dimensions, provided that the size of the longer side is larger than the size of the shorter side.

According to the form of the element according to the invention the target ion sputtering of the Moo2or containing MoO2attached to the base plate to form a target ion spray a large area. In a specific embodiment, the invention may be used a method of spray forming segments.

Spray the plate with a large area can be any suitable shape and size. As a non-limiting example, the spray plate of large area can be in the shape of a square, rectangle, circle or oval. In the special the practical embodiment of the invention the square of the sprayed plate can be square and have dimensions of 0.1 m × 0.1 m to 6 m × 6 m, in some cases, from 0.5 m × 0.5 m to 5.5 m × 5.5 m, in other cases from 1 m × 1 m to 4 m × 4 m, in some situations, the 2 m × 2 m to 3 m × 3 m, and in other situations square spray plate has dimensions of about 2.5 m to about 2.5 m

Rectangular spray plate large area may have a length of a shorter side of at least 0.1 m, in some cases at least 0.5 m, in other cases at least 1 m, in some situations at least 2 m, in other situations at least 2.5 m, in some examples at least 3 m, in other examples, at least 4 m, in specific situations, at least 5 m, and in specific examples, at least 5,5 m Also longer side of the rectangle can be up to 6 m in some cases, up to 5 m, in other cases up to 4 m, in some situations up to 3 m, in other situations up to 2.5 m, in some instances up to 2 m, in other instances up to 1 m, and in the specific examples to 0.75 M. the dimensions of the rectangular spray plate large area can vary between any of the sizes specified above, provided that the size of the longer side is larger than the shorter side.

Film in the optical display device is formed using one or more methods selected from the group consisting of ORGANOMETALLIC chemical osai the texts from the vapor phase (MACHOP), metal-organic deposition (LEAs) and Sol-gel method.

As used here, MOHOP or ORGANOMETALLIC chemical vapor deposition" refers to a method of increasing the film by chemical vapor deposition, in which all the materials to be deposited are present in the gas phase above the surface of the deposition. In MOHOP sources of chemical deposition from the vapor phase are ORGANOMETALLIC compounds that have oxygen as a heteroatom, to bind metal atom with one or more organic ligands. As a non-limiting example ethylhexanoate, molybdenum may be used as the ORGANOMETALLIC precursor for the production of thin films of Moo2. As a specific non-limiting example, the precursor can be contained in a boat made of quartz glass or in a reaction tube made of quartz glass, and these compounds is heated to a temperature close to the boiling point, after which it is introduced as a carrier gas argon with a suitable partial pressure of oxygen to oxidize this compound in a reducing atmosphere to obtain molecules of Moo2and then precipitate on the substrate in the reaction chamber.

Used herein, "Sol-gel process" refers to treatments is ke using alkoxides of metals, forming a grid of cations as the precursor solution. As a non-limiting example, the cations can be represented as M(OR)xwhere M represents a metal, a R is an alkyl group. In addition to this example, the source alkoxide to obtain MoO2the Sol-gel process can be a molybdenum acetylacetonate (in methanol). The hydrolysis can then be carried out by combining the solution with ethyl alcohol to obtain the polymerized solution. The precursor solution is stable for only a few days, after which the transparency is lost, and may come gelation. The precursor solution may be applied onto the substrate, followed by centrifugation at, e.g., 1000 rpm, to obtain a thin wet film. Another method of manufacturing a thin film consists of immersion of the substrate in the precursor solution using the rate of withdrawal, for example, 580 mm per minute. Wet film can then be thermally treated in vacuum and hydrogen atmosphere (reducing atmosphere) to obtain a thin film of Moo2on the substrates.

Used herein, the terms "process of the IPO" or the "process of ORGANOMETALLIC deposition" refers to the processes that are similar to the processes MO the OP and/or Sol-gel. In the process of the NGO are also using ORGANOMETALLIC compounds as precursors, which have oxygen as heteroatom binding of the metal atom with one or more organic ligands. These compounds are dissolved in suitable solvents, and non-limiting example is xylene. As a non-limiting example of the ORGANOMETALLIC compound can be used ethylhexanoate, molybdenum or molybdenum acetylacetonate, to obtain a thin film MoO2. After the establishment of the rheology of the solution forming the liquid film forming precursor solution on the substrate.

Usually the last stage in the process of the IPO is pyrolysis, which involves evaporation of the solvent, thermal decomposition of compounds and solid solution with the formation of the film MoO2in the corresponding oxidizing and reducing atmosphere.

In the embodiment of the invention in the process of the IPO in addition to a thin film of pure phase MoO2can also be obtained film containing the Moo2by mixing several different solutions of ORGANOMETALLIC compounds. As a non-limiting example miscible ethylhexanoate molybdenum with ethylhexanoate tin in a solvent such as xylene, in relation to p and which achieves the desired stoichiometry. After molding to obtain a wet film on the substrate carry out the pyrolysis at a suitable partial pressure of oxygen to produce a thin film of molybdenum oxide and tin (film containing MoO2).

In the embodiment of the invention methodology, MOHOP or LEAs using ORGANOMETALLIC chemical compounds, including ethylhexanoate molybdenum.

In the embodiment of the present invention a thin film in the present optical device may have a work function of 4.5 to 6 eV, in some cases, from 4 to 5.5 eV, and in some situations from 4.5 to 5.5 eV. In another embodiment of the present invention a thin film can typically have a roughness of less than about 5 nm, in some cases, from 0.1 nm to 5 nm, and in other cases from 0.1 to 2.5 nm.

In the following embodiment of the present invention a thin film can have an average transmittance over 85%, in some cases, more than 90%, and in other cases more than 95% at a wavelength of from 350 nm to 800 nm.

In an additional embodiment of the invention, a thin film may have a resistivity less than 300 µohm×cm, in some cases less than 250 µohm×cm, and in other cases less than 200 µohm×see

The optical device may be an organic light emitting diode, and a film containing MoO2that is the anode, when the volume of the organic light emitting diode includes:

(a) a metal cathode;

(b) electron transport layer;

(C) an emitter layer;

(d) a hole transport layer;

(d) a film comprising the Moo2as the anode layer.

In some aspects of this variant of the invention, the thin film may be located on a substrate selected from plastic substrates, glass substrates, ceramic substrates, and combinations thereof. As a non-limiting example, the plastic substrate may include one or more plastics selected from polynorbornene, polyimide, polyarylate, polycarbonate, polyethyleneamine and polyethylene terephthalate. Also, as a non-limiting example, the ceramic substrate may include a sapphire.

In another embodiment of the invention, the optical device is a light emitting diode and a thin film containing the Moo2may be an ohmic contact. Further, in this embodiment of the invention, the light emitting diode may include:

(a) a substrate;

(b) a buffer layer;

(in) the semiconductor material is N-type;

(g) a p-n transition layer;

(d) semiconductor material is P-type;

(e) a metal contact to p-type;

(g) a metal contact to n-type.

Non-limiting examples of suitable substrates are those in luchot material, selected from sapphire, SiC, Si, GaN, GaP, GeSi, AlN, and combinations thereof. Non-limiting examples of suitable materials for the buffer layer are those which contain one or more compounds of elements of group IIIB and the elements of group VB of the periodic table of elements. Used herein, the term " periodic table of the elements" refers to the format of the periodic table, used by IUPAC. In a specific embodiment of the invention, the buffer layer comprises AlN, GaN, or a combination thereof.

In another aspect, the variant of the invention, the light-emitting diode is a semiconductor material of N-type may include, but are not limited to, materials containing one or more compounds, doped with one or more elements selected from Si, Se, Te and S. non-limiting examples of such compounds include compounds of elements of group IIIB and the elements of group VB of the periodic table of elements and compounds selected from compounds of elements of groups IIB and elements of group VIB of the periodic table of elements. Non-limiting examples of suitable compounds of elements of group IIIB and the elements of group VB include doped Si compounds selected from GaN, GaAs, GaAlAs, AlGaN, GaP, GaAsP, GaInN, AlGaInN, AlGaAs, AlGaInP, PbSnTe, pbsnse heterostructure lasers and their combinations. Non-limiting examples of suitable compounds of elements of groups IIB and elements of group IB include doped Si compounds, selected from ZnSSe, ZnSe, SiC, and combinations thereof.

In another aspect, the variant implementation of the light-emitting diode according to the invention a thin film may be a metal contact to n-type. In specific embodiments the invention, the metal contact n-type may include a material selected from metals of Ti/Au, conductive oxide of Moo2and MoO2/metal, where the metal is selected from Ti, Au, and combinations thereof.

In another aspect, the variant implementation of the light-emitting diode according to the invention, semiconductor material is P-type may include one or more compounds, doped with one or more elements selected from Mg, Zn and S. Suitable connections in this aspect of the invention include compounds of elements of group IIIB and the elements of group VB of the periodic table of elements and compounds selected from compounds of elements of groups IIB and elements of group VIB of the periodic table of elements. Non-limiting examples of suitable compounds of elements of group IIIB and the elements of group VB include Mg-doped compounds selected from GaN, GaAs, GaAlAs, AlGaN, GaP, GaAsP, GaInN, AlGaInN, AlGaAs, AlGaInP, PbSnTe, pbsnse heterostructure lasers and their combinations. Non-limiting examples of suitable compounds of elements of groups IIB and elements of group VIB include Mg-doped compounds selected from ZnSSe, ZnSe, SiC, and combinations thereof.

In another aspect of the variations is that the implementation of the light-emitting diode according to the invention a thin film may be a metal contact to p-type. In specific embodiments the invention, the metal contact p-type includes a material selected from transparent conductive oxide containing MoO2and films containing the Moo2/metal, where the metal is selected from Ag, Au and combinations thereof.

In the embodiment of the invention, the optical device may be a liquid crystal display and thin film containing the Moo2represents one or more of the following: common electrode, pixel electrode, gate electrode, source electrode, drain electrode, electrode storage capacity and their combinations. In addition to this variant of the invention, the liquid crystal display may include a thin-film diode or a thin-film transistor element of the switch.

Aspects variant of the invention, the liquid crystal display includes liquid crystal displays, which include:

A) glass substrate,

B) a source electrode,

B) a drain electrode,

G) gate dielectric,

D) electrode of the gate,

E) a layer of amorphous silicon, polycrystalline silicon or single crystal silicon,

G) a layer of n-doped silicon,

C) a passive layer

And the transparent pixel electrode

To the common electrode,

L) a polyimide orientation layer,

M) electrode storage capacity.

In some aspects of this variant of the invention, the transparent pixel electrode and the common electrode may include a film containing the Moo2.

Another variant of implementation of the present invention is directed to the situation where the optical device is a plasma display panel, and a film containing the Moo2represents the positive or negative electrode. In this embodiment of the invention a plasma display panel may include:

A) front glass plate,

B) a dielectric film,

B) a layer of MgO,

D) ionized gas,

D) a separator,

E) one or more phosphors,

W) of the rear glass plate.

In some aspects of this variant of the invention, the rear glass can be coated with a thin film of Moo2.

Further embodiments of the invention are directed to situations where the optical device is a display with autoelectronic emission, and a thin film containing MoO2represents the electrode material of the anode or cathode. In this embodiment of the invention the display autoelectronic emission may include:

A) glass front plate anode,

B) phosphor,

B) a spacer,

D) micro is the PLU g connector,

D) horizontal and vertical cathodes,

E) glass carrier plate.

In some aspects of this variant of the invention, the glass face plate And coated with a thin film containing MoO2. In another aspect of this variant of the invention, at least one of the horizontal and vertical cathodes D) may include a thin film containing the Moo2.

In an additional embodiment of the invention, the optical device may be a solar cell, and the film containing the Moo2may be one or more of the following: electrical contacts, a transparent contact and the upper p-n transition layer. In this embodiment of the invention, a solar cell may include:

A) coating a glass,

B) the top electrical contact layer,

B) transparent contact

G) the upper p-n transition layer,

D) an absorbent layer,

E) back electrical contact,

W) substrate.

In some aspects of this variant of the invention, the transparent contact) may include a film containing the Moo2. In another aspect of this variant of the invention, the upper p-n transition layer D) may include a film containing the Moo2. The following aspect of this variant implementation invented the I cover glass And may include anti-reflective coating.

Examples

Example 1

Four different powder MoO2were characterized regarding their behavior during sintering and shrinkage by using a dilatometer. Small samples of about ⌀8×10 mm was pressed steel die and then condensed in a cold isostatic pressing (HIP). Four powder MoO2showed the following characteristics:

Powders MoO2used for experiments seal

DesignationThe dirt content, ppmSpecific surface area m2/gMineralogical phase
IPO-R 1>1000,5Moo2
IPO-R 2<501,0MoO2,
MoO2traces Mo4O11
IPO-R 3<502,3Moo3
IPO-R 4<502,0 MoO2

When heated with a rate of 5K/min to 1250°C in an atmosphere of Ar-3H2in the dilatometer samples made from LEAs-R 1, 2 and 4, showed reduced expansion and compaction and reached a density comparable with the initial density immediately after pressing" about 3.5 g/cm3. In contrast, a sample made from LEAs-R 3, showed initial shrinkage at about 600°C, which continued until the maximum temperature of 1250°C. Fixed shrinkage amounted to 10.3%, the measured density after the experience in the dilatometer was 4.1 g/cm3.

These results are interpreted by the fact that the content of impurities or surface area of the powders does not have a significant impact on behavior when the seal is in contrast to the mineralogical phases.

Example 2

Samples of about ⌀30×5 mm were obtained in the same manner as described in test 1, IPO-R from 1 to 4. Density immediately after pressing" was about 3.5 g/cm3. These samples were specaly in gas-tight lined Al2O3furnace in an atmosphere of Ar-3H2placed on the recrystallized SiC plate. Co a heating rate of 5°K/min the temperature was raised to 1100, 1150, 1200, 1250 and 1300°C, respectively, followed by from 1 to 5 h time of impregnation. Up to 1200°C could be defined weak increase densely the tee after the sintering cycle to a density of about 3.8 g/cm 3except for the samples made from LEAs-R 3, which reached a density of up to 4.1 g/cm3. Further increase in temperature led again to low densities and increase weight loss. These results are again interpreted by the fact that the content of impurities or the specific surface area of powders do not have a significant impact on behavior during sintering unlike mineralogical phases.

Example 3

Powder LEAs-R 4 was placed in a lined foil from Mo mold for hot pressing, made of graphite. Various tests of the hot pressing was carried out at increasing temperatures ranging from 750, 1000 and finally, 1300°C. the Maximum pressure of 30 MPa was applied at 600°C, to give a series of hot pressing, when the dilatometer was registered seal as a function of temperature. The rate of heating and cooling was 10 K/min, while used again the atmosphere of Ar-3H2. None of these conditions did not lead to a strong, tight pattern. Basically, it was destroyed during ejection from the mold and was so soft that scratching by nail. When tested at 1300°C have been serious reaction with foil Mo, which led to strong adhesion.

Thus, the powder is not suitable for sealing when technically feasible, the services is established by hot pressing.

Example 4

IPO-R 4 was mixed with 2.5 wt.% fine powder of Moo3. Mixing was performed on Katkova frame for 5 hours inside the plastic container in a dry condition, using the balls of Al2O3for allocation. The mixed powder was sieved by taking the fraction of <300 μm, and used for further testing of hot pressing. The maximum pressure of 30 MPa was applied at 600°C, to give a series of hot pressing, when the dilatometer was registered seal as a function of temperature. The rate of heating and cooling was 10 K/min, while used again the atmosphere of Ar-3H2. The system logs the beginning of seals at about 700°C, which lasted until about 800°C. Further increase in temperature did not lead to further compaction. After popping has determined that the density was about 5.9 g/cm3. Not was no reaction with the insulating foil from Mo. According to x-ray diffraction could only be detected phase MoO2. There were no signs of the presence of crystalline phases of Mo with respect to O/Mo>2 is above the limit of detection by x-ray diffraction. This supports the conclusion that a few percent of the phases of Mo with respect to O/Mo>2 can be compacted powders of Moo2(inside the specification limits, indicated the data above) by hot pressing up close to theoretical density at relatively low temperatures.

Example 5

In order to analyze the influence of the quantity added of Moo3the compacting of the powder MoO2when hot pressing, NGO-R 2 was mixed with 2, 3 and 5 wt.% powder of Moo3accordingly, counting in test 4. Conditions of hot pressing was established the following: 750°C, the time of soaking for 30 minutes, a pressure of 30 MPa and atmosphere of Ar-3H2. As an insulating foil used graphite.

Under these conditions the sample #1 with 1 wt.% supplements of Moo3reached a density of 4.5 g/cm3, while sample #2 with 3 wt.% and sample #3 with 5 wt.% supplements of Moo3reached a density of 6.1 g/cm3. There was no indication of a reaction between the sample material and graphite insulating foil. These samples were solid and could not be scratched with a fingernail. According to x-ray diffraction could only be detected phase MoO2, there were no indications of the presence of crystalline phases of Mo with respect to O/Mo>2 is above the limit of detection by x-ray diffraction.

Adding 3 wt.% Moo2in accordance with the procedure described in test 4, and under conditions of hot pressing, similar to above, but with longer times of impregnation could be obtained plates with densities >6.0 g/cm3with ⌀ 50-250 mm and a thickness of up to about 20 mm, Thus, this procedure p is hodna to obtain a plate of Moo 2high density with dimensions that have a technical interest.

This invention and the various options for its implementation described above. It will be obvious to experts in the art that various changes and modifications can be made therein without departing from the scope of the invention, which is defined in the description and the attached claims.

1. Powder of Moo2containing more than 99% of the stoichiometric amount MoO2.

2. A method of manufacturing a wafer, including:
(a) isostatic pressing component of more than 99%of stoichiometric powder of Moo2in the workpiece;
(b) sintering in vacuum this procurement under the conditions of maintaining over 99%stoichiometry MoO2;
(C) forming plate, comprising more than 99% of the stoichiometric MoO2.

3. The method according to claim 2, where the workpiece is sintered in vacuum for 6 hours at a temperature of at least 1250°C.

4. The method according to claim 2, where the powder MoO2is subjected to isostatic pressing at a pressure in the range from 68,95 MPa (10000 psi) to 275,79 MPa (40000 pounds per square inch).

5. The method according to claim 2, where the plate is subjected to hot isostatic pressing.

6. The method according to claim 2, where the plate has a density that ranges from 90 to 100% of theoretical density MoO2.

7. Method of atomization, in which the plate containing more than 99% of the stoichiometric MoO2expose the conditions of spray.

8. The method according to claim 7, where the sputtering is conducted using the atomization method selected from the group consisting of magnetron sputtering, pulsed laser sputtering, ion beam sputtering, triode sputtering, and combinations thereof.

9. The method of manufacturing a thin film, comprising the steps:
(a) spraying plate, containing more than 99% of the stoichiometric MoO2;
(b) removing molecules of Moo2with the plate; and
(C) applying the molecules of Moo2on the substrate and thereby form a thin film.

10. The method according to claim 9, where the thin film has a thickness ranging from 0.5 nm to 10 microns.

11. The method according to claim 9, where the atomization method selected from the group consisting of magnetron sputtering, pulsed laser sputtering, ion beam sputtering, triode sputtering, and combinations thereof.

12. The element includes a sputtering target, the sputtering target includes machined plate of MoO2high purity obtained by the method according to claim 2.

13. Item by item 12, where the plate is processed using the methods of laser cutting, milling, tilting or machining on a lathe.

14. Item by item 12, where the target has a thickness in the range from about 0.15 cm to about 20 cm

15. A method of manufacturing a plate, in which a component consisting of a powder containing more than 99% of the stoichiometric MoO2process in the conditions of hot pressing forming plate, comprising more than 99% of the stoichiometric NGO2.

16. The method according to clause 15, where the hot pressing is carried out with a transition in the liquid phase, contributing to hot pressing.



 

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