Levelling film and method of its operation

FIELD: process engineering.

SUBSTANCE: invention relates to production of sandwiched materials used in thin-film instruments and devices. Proposed levelling film comprises levelling ply containing binding polymer resin and inorganic filler as components, at least, on one side of transparent polymer substrate. Note here that the number of foreign particles with mean diameter of 20-100 mcm on levelling air surface does not exceed 5 per m2.

EFFECT: decreased amount of linear defects at production of thin-film transistor on film surface.

3 cl, 1 tbl, 3 ex, 2 dwg

 

The technical field to which the invention relates.

The present invention relates to a leveling film. This invention relates in particular to the alignment film, suitable for the substrate in the thin film transistor. More specifically, the present invention relates to a leveling film suitable for use in thin film transistors (hereinafter sometimes referred to as TFT (TFT), such as organic thin-film transistors (OTPT (OTFT)), transistors made of amorphous silicon (a-Si TFT (a-Si TFT)and the transistors of crystalline silicon and thin-film devices, a variety of displays, electroluminescent (EL) displays, liquid crystal displays, electrochromic devices, and the like, and to a method of manufacturing such a film.

The level of technology

In recent years, instead of paper as a material for presenting images on the display active development of flexible electronic materials for displays such as electronic paper (E-paper and flexible displays, and it is expected that these materials will be used in electronic devices for reading books (e-books, e-Newspapers, etc. Used in such electronic display devices should be flexible; examples of such devices include electrophoretic displays and flexible organization is a mini electroluminescent device. Thus, the development of flexible devices used polymeric film substrate instead of the previous glass substrate (Patent documents 1-3). In addition, to control the flexible display must be created on the polymer film substrate thin-film transistors for the manufacture of thin-film devices (Patent documents 4 and 5). In addition, the polymer film substrate, in General, more permeable to gases than the glass substrate, which gives rise to the problem lies in the fact that thin-film device using the polymeric film substrate, is more susceptible to degradation. As a result, considered the use of gas-tight layer on the polymeric film substrate to prevent such degradation (Patent documents 6 and 7). Thus, previously performed a number of studies in the field of flexible displays.

(Patent document 1) JP-A-2008-49695.

(Patent document 2) JP-A-11-348189.

(Patent document 3) JP-A-2007-152932.

(Patent document 4) JP-A-2007-311377.

(Patent document 5) JP-A-2008-147346.

(Patent document 6) JP-A-2005-288851.

(Patent document 7) JP-A-2006-95783.

Disclosure of inventions

At the same time, if you perform a thin-film transistor directly on the polymeric film substrate, it is possible faults and failures so what about the thin-film transistor due to the influence of the surface of this polymer film substrate. Thin-film transistor includes transistor devices, each of which corresponds to one pixel, is made on top of the device, and the lines of the source electrode or the drain electrode of such transistor device shared transistor devices arranged in the longitudinal or in the transverse direction of the screen. Consequently, in the event of termination of this line in one transistor device this defect causes a failure of all of the transistors located in the specified longitudinal or transverse direction of the screen (linear defect). In such case, of course, the device in such a thin-film transistor also fails, so it becomes a "fatal" problem for a commercial product.

Therefore, the first aim of the present invention is to provide a leveling film, which when used for thin-film transistor substrate capable of preventing the formation of linear defects even in the case of forming a thin film transistor directly on this tape.

The second objective of the present invention is to provide a manufacturing method to consistently generate such a leveling film.

The above first objective of the present invention can be achieved by using the leveling film comprising virani the surrounding layer, containing binder polymer resin and inorganic filler as components, at least one side of a transparent polymer base. This alignment layer is characterized by the fact that the number of foreign particles with an average diameter ranging from 20 μm to 100 μm on the surface layer does not exceed 5/m2.

The above second objective of the present invention can be achieved by using the method of manufacturing the alignment film, comprising applying a liquid coating to the surface of the transparent polymer bases for the formation of the alignment layer, and the specified liquid coating is obtained by adding a binder polymer resin and the inorganic filler in a solvent and mixing. The method differs in that the liquid coating has a concentration of solids of 25% to 45% by weight, and the liquid coating is applied using an engraved cylinder with density lines 50-90 lines/inch and the rate of rotation of 60-100%, and the coating is dried/utverjdayut for the formation of the alignment layer.

Brief description of drawings

Figure 1 is a sectional view of the example of the alignment film according to the present invention.

Figure 2 is a sectional view of the thin-film transistor is performed on the alignment film, serving p is the iMER according to the present invention.

Digital RefDes

1 Transparent polymer base

2 Levelling layer

3 Easy glue layer

4, 5, the source Electrode or the drain electrode

6 Organic semiconductor layer

7 Insulating layer

8, the gate Electrode

9, a Protective layer

The implementation of the invention

[Leveling tape]

A leveling film comprises discussed below levelling layer at least on one side, considered below, a transparent polymer base.

[Transparent polymer base]

The choice of design and materials transparent polymer base with respect to the present invention does not specifically limited. Examples of such bases include plates and film made of polyester materials such as polyethylene terephthalate and polyethylene naphtalate, polyolefin materials, such as polycarbonate, polyethylene and polypropylene, polystyrene triacetyl cellulose, acrylates and the like, In particular, on the basis of the excellent optical properties such as transparency, mechanical properties and heat resistance, as well as in connection with a good ratio between performance and price, it is preferable to use a polyester film, and in General, preferred are films of polyethylene terephthalate or polyethylene naphthalate. As such, the film is even more preferable to use a biaxial stretched film, because it has a higher optical properties, mechanical properties and heat resistance.

Transparent polymer base according to the present invention preferably essentially does not contain particles of a lubricant (for example, not more than 0,004% and preferably not more than 0.001% by weight of a transparent polymer base). When the material is essentially no lubricant particles can be easier to implement specified by the present invention features on the content of foreign substances. In addition, achieved an excellent transparency.

The thickness of the transparent polymer base does not specifically limited. However, in the interests of achieving excellent optical properties and workability, the thickness should preferably be in the range of 25-300 μm, more preferably in the range of 50-200 μm, and particularly preferably within 75-188 microns.

The surface of the transparent polymeric base according to the present invention may be specially treated to improve adhesion of the alignment layer, for example by creating easily glued layer by corona treatment, etc. as such easily glue layer as the preferred example may be specified layer, anchor coating described, e.g. the measures in Applications for the Japan patent JP-A-2007-216610 or JP-A-2007-206316.

[Leveling layer]

The alignment layer according to the present invention contains, as components of the binder polymer resin and inorganic filler.

According to the present invention such a leveling layer, perform at least one side of a transparent polymer base to compensate for defects the surface of this transparent polymer base, such as scratches and particles, thereby creating the alignment film with a high degree of flatness of the surface. To obtain a high degree of flatness of the surface on the level attainable in accordance with the present invention, it is important to exercise strict control method of manufacturing the alignment layer in addition to the selection of materials for the manufacture of this leveling layer. Details will be discussed later.

(Foreign particles on the surface of the alignment layer)

In the alignment layer according to the present invention, the number of foreign particles with an average diameter (defined as the average of the four values for a single particle: the largest diameter of the particles, the length of the particle in the direction perpendicular to the greatest diameter, and length of the particles in directions at angles of ±45° to the greatest diameter) is 20 μm to 100 μm is less than 5/m 2. With such parameters foreign particles on the surface of the alignment layer provides excellent flatness. The notion of "particles" in the description of the invention comprises particles of foreign origin, who are in the leveling layer in the process of its manufacture (during the coating process and the like), particles of the composition of the liquid coating used to create the alignment layer, particles of the composition of the transparent polymer base, as well as sinks in the surface of the alignment layer, which may be associated with the influence of such particles. In particular, the authors of the present invention found that when the thin film transistor directly on the surface of the alignment layer, if the number of particles specified average diameter of from 20 μm to 100 μm) is within the specified range (no more than 5/m2), defects such thin-film transistors cannot sufficiently be avoided. In other words, the authors of the present invention found that there is a particularly strong correlation between the failures of thin-film transistors and the presence of foreign particles of some specific average diameter, and also found that by controlling the number of such particles can sufficiently pre order to prevent malfunction of the thin-film transistor. The number of such particles preferably should not exceed 4/m2even more preferably should not exceed 3/m2and particularly preferably should not exceed 2/m2that will help even more to reduce the probability of failure of thin-film transistors. Such content particles cannot be achieved by simply increasing the purity of the process. The authors of the present invention have achieved a situation with foreign particles, having picked up the first optimal liquid coating for formation of the alignment layer, and having found the optimal way to create a layer (method of coating).

The following describes other preferred elements of the alignment layer together with the components that make up this leveling layer, and a method of creating a layer to achieve the above, the content of particles.

(The average roughness of the surface of the alignment layer on the middle line)

For the alignment layer according to the present invention, it is preferable that the upper limit of the average surface roughness of the center line (Ra) did not exceed 10 nm. If the roughness Ra of the surface of the alignment layer is in the above range, created on this layer thin-film transistor has a uniform thickness of the inu. If the roughness Ra is too large, the thickness of the thin-film transistor made on this surface becomes uneven. From this viewpoint, the upper limit of the roughness Ra even more preferably should be not more than 5 nm and especially preferably not more than 2 nm. At the same time, if we talk about the lower limit of the roughness Ra, smaller values are more preferable, but the practical lower limit is not less than 0.1 nm.

The above values of the roughness Ra can be achieved by adequate selection of the thickness of the alignment layer or of the average particle size and content of the lubricant particles in a transparent polymer base. For example, there may be used the preferred range according to the present invention.

(The thickness of the leveling layer)

The thickness of the alignment layer according to the present invention preferably is in the range from 3 μm to 8 μm, still more preferably from 4 μm to 7.5 μm, and particularly preferably from 5 μm to 7 μm. When the thickness of the leveling layer is within the specified limits, the effect of improving the flatness can be enhanced. Moreover, it is possible to prevent warpage. When the thickness is too small, it becomes difficult to close the scratches, particles and other defects on the surface of the transparent polymer substrate, the bumps n the surface or similar defects, so the effect of improving the flatness may be impaired. At the same time, when the thickness is too large, the mechanical stress of shrinkage in the leveling layer that occurs when heated in the manufacturing process of thin-film transistors become too strong, so that the alignment layer has a tendency to warping.

[Components forming the alignment layer]

The alignment layer according to the present invention contains, as described above, the binder polymer resin and the inorganic filler as the component. In the framework of the present invention the binder is a polymer resin and inorganic filler are used together (hybridizing) as components forming the alignment layer. As a result, in the process of applying liquid coatings to create the alignment layer, it is possible to prevent foreign particles generated during the shearing tool for applying coating that helps to reduce the average diameter of these particles and the number of generated particles. In addition, this method allows you to create a levelling layer with high surface hardness and strength.

Next will be described the components forming the alignment layer according to the present invention.

(Binder polymer resin)

Swazey the traveler polymer resin according to the present invention contains mainly the composition based on radiation-curable polymer resin.

Such radiation-curable polymer composition is a monomer, oligomer or polymer, curable by radiation. Specified radiation-curable polymer composition according to the present invention is preferably a polyfunctional (meth)acrylate compound such as a polyfunctional (meth)acrylate monomer, a polyfunctional (meth)acrylate oligomer or polyfunctional (meth)acrylate polymer, resulting in the cross-linking density after curing can be increased and can be achieved a higher surface hardness and strength, so that you can maintain the flatness of the alignment layer, as well as to achieve greater transparency.

Mentioned polyfunctional (meth)acrylate compound is a compound having in a molecule with (meth)acridology group, and preferably, this connection was in the molecule at least two (meth)acryloyloxy group. This structure promotes the formation of cross-linkages (linkage) in the radiation-curable resin composition, allowing you to obtain a higher surface hardness and strength. In addition, this reduces the likelihood of deformation of the surface under the influence of external forces, and other such factors that POS is s to maintain the flatness of the alignment layer. Polyfunctional (meth)acrylate compound according to the present invention may have other curable functional group in the molecule in addition to the (meth)acryloyloxy groups.

Specific examples of the polyfunctional (meth)acrylate compounds having in a molecule at least two (meth)acryloyloxy group include neopentyl glycol di(meth)acrylate, trimethylol propane three(meth)acrylate, pentaerythritol three(meth)acrylate, trimethylated three(meth)acrylate, pentaerythritol Tetra(meth)acrylate, dipentaerythritol Tetra(meth)acrylate modified with alkyl dipentaerythritol Tetra(meth)acrylate, dipentaerythritol Penta(meth)acrylate modified with alkyl dipentaerythritol Penta(meth)acrylate, dipentaerythritol hexa(meth)acrylate, modified caprolactone dipentaerythritol hexa(meth)acrylate, ditrimethylol Tetra(meth)acrylate and melamine meth(acrylate), and a monomer for about 20-dimensional oligomers at one of these compounds and polymers of at least one of these compounds. In the present invention can be used such polyfunctional (meth)acrylate compound of only one type, but can also be used in a similar connection of two or more kinds together.

On sale are such polyfunctional (meth)acrylate compounds containing p is at least two (meth)acryloyloxy group, for example the following brands Aronix M-400, M-450, M-305, M-309, M-310, M-315, M-320, TO 1200, TO-1231-595, TO-756 (all produced by the company Toagosei), KAYARD D-310, D-330, DPHA, DPHA-2C (all produced by the company Nippon Kayaku) and NIKALAC MX-302 (manufactured company Sanwa Chemical).

(The initiator of photopolymerization)

Further, according to the present invention to create a leveling layer with improved surface hardness and durability, it is preferable to use the initiator of photopolymerization. Excellent surface hardness and strength help to maintain the flatness of the alignment layer. Examples of such photopolymerization initiators include 1-hydroxycyclohexyl phenyl ketone, 2,2-dimethoxy-2-phenylacetophenone, xanthone, fluorenone, anthraquinone, benzaldehyde, fluorene, anthraquinone, triphenylamine, carbazole, 3-methylacetophenone, 4-chlorobenzophenone, 2,2-dimethoxy-2-phenylacetophenone, 2-methyl-1-1[4-(methylthio)phenyl]-2-morpholino-propane-1-he, 2,4,6-trimethylbenzoyl diphenylphosphine oxide and bis-(2,6-dimethoxybenzoyl)2,4,4-trimethylpentyl phosphine oxide.

According to the present invention, the photopolymerization initiator of the added preferably in an amount of from 0.1% to 10% by weight, taking the weight of the binder polymer resin for 100%. When the number of added initiator is within the specified limits, it is possible to achieve a higher surface hardness and strength. In addition, easier to maintain is giving the flatness of the alignment layer. If the number of added initiator is too large, the added initiator of photopolymerization acts as a plasticizer, which may reduce the effect of improving the flatness implemented a levelling layer. In addition, can reduce the surface hardness and strength.

(Inorganic filler)

The alignment layer according to the present invention contains an inorganic filler to reduce the average diameter or the number of foreign particles on the surface of the alignment layer to improve the flatness, increase surface hardness and strength, increase transparency, or prevent wrinkling.

As such inorganic filler is preferable to use silicon oxide or aluminum oxide, which reduces the average diameter and the number of foreign particles on the surface of the alignment layer, which in turn contributes to improved flatness. In addition, it is possible to achieve greater transparency. In particular, it is preferable to use silicon oxide, which allows you to make the average diameter and the number of foreign particles on the surface of the alignment layer is particularly small, and this in turn makes it possible to achieve a high degree of flatness.

According to the present invention mentioned above neorg the organic filler may be added to reduce the average diameter and the number of foreign particles on the surface of the alignment layer and thereby improving the flatness. However, you should choose the inorganic filler, which would not affect the optical properties of the alignment film according to the present invention. For example, it is preferable to use the inorganic filler, the average particle size and the refractive index of which lie within the given ranges.

To achieve the above purposes, the average particle size of the inorganic filler should preferably be in the range from 2 nm to 2000 nm. The use of material with an average particle size in the above range can reduce the average diameter and the number of foreign particles, to improve the flatness and increase surface hardness and rigidity while maintaining transparency of the alignment layer. When too large an average particle size of the inorganic filler layer transparency is reduced. In addition, the average diameter or the number of particles is likely to increase. At the same time, when the average particle size is too small, the strength of the inorganic filler is reduced, which leads to a decrease in surface hardness and strength of the layer. In addition, the effect of improving the flatness becomes weaker. From this viewpoint, the average particle size of the inorganic filler is more preferably should be in the range from 3 nm to 20 nm, and particularly preferably in the range from 5 nm to 100 nm.

Further, it is preferable to use an inorganic filler with a specific refractive index, i.e. it is preferable to use inorganic fillers, the refractive indices are different from the refractive index of a binder polymer resin is less than 0.1. If the difference of the refractive index is in the above range, it becomes easier to maintain the transparency of the alignment layer even when adding inorganic filler. As a consequence, it becomes easier to provide the preferred average particle size and the number of such particles, which reduces the average diameter and the number of foreign particles, to improve the flatness and increase the surface hardness and strength. If the difference of the refractive index is too large, the transparency of the layer decreases. From this point of view, the difference between the refractive preferably should be less than 0.08 and even more preferably less than 0,06.

In addition, the content of the inorganic filler should preferably be in the range from 10% to 250% by weight, taking the weight of the binder polymer resin for 100%. If the content of the filler lies in the above range, it is possible to reduce the average diameter and the number of foreign particles, to improve the flatness and increase the th surface hardness and rigidity while maintaining transparency of the alignment layer. When the content of the filler is too large, the average diameter and the number of foreign particles, likely increases. Moreover, transparency is reduced. When the content of the filler is too small, the effect of improving the flatness is weaker. When the surface hardness and strength of the layer is also reduced. From this point of view, the content of the filler is more preferably should be in the range from 40% to 100% by weight, taking the weight of the binder polymer resin for 100%.

In the present invention can be used inorganic filler only one species, or to apply a combination of two or more kinds of inorganic fillers.

According to the present invention, it is preferable to use the inorganic filler in the form of powder or dispersion Zola, obtained by dispersion of a powder of inorganic filler in the solvent for the formation of Zola. When the inorganic filler is used in the form of a dispersion or Sol, as a dispersing medium, it is preferable to use an organic solvent from the viewpoint of improving compatibility with the binder polymer resin. Examples of such organic solvents include alcohols, such as methanol, ethanol, isopropanol and butanol; ketones, such as acetone; methyl ethyl ketone, methyl Isobe is Il ketone and cyclohexanone; esters, such as ethyl acetate, butyl acetate, propylene glycol monomethyl ether acetate and propylene glycol monoethyl ether acetate; ethers such as propylene glycol monomethyl ether and propylene glycol monoethyl ether; and aromatic hydrocarbons such as benzene, toluene and xylene. In particular, preferred are methanol, isopropanol, butanol, methyl ethyl ketone, methyl isobutyl ketone, ethyl acetate, butyl acetate, toluene, and xylene, which allows to achieve excellent compatibility. In addition, to improve the dispersive ability of the pigment inorganic filler can be added various surfactants, amines, etc.

As such inorganic fillers can preferably be used, for example, oxides of silicon in the form of a dispersion of colloidal solution present in the market under the brand names of IPA-ST, MEK-ST, NBA-ST, XBA-ST, DMAC-ST, ST-UP, ST-OUP, ST-20, ST-40 (all of these materials produces Nissan Chemical Industries), and others. Alternatively, it is preferable to use aluminum oxide in the form of a dispersion of colloidal solution present in the market under the brand names ALUMINASOL-100, ALUMINASOL-200, ALUMINASOL-500 (all of these materials produces Nissan Chemical Industries), AS-150I, AS-150T (all of these materials produced by the company Sumitomo Osaka Cement) and others.

In addition, the surface of the inorganic filler according to the present invention preferably processed is polymerized with the compound for surface treatment to improve the dispersive ability of the pigment in the binder polymer resin, to achieve a well-dispersed state in the leveling layer or to create the stitching point in the binder polymer resin to improve surface hardness and strength of the alignment layer.

As such compounds for surface treatment is preferable to use, for example, a compound containing a group of silanol, or forming such group by hydrolysis (hereinafter sometimes also referred to as Celanova binding agent). In addition, it is preferable to use a silane bonding agent containing a group of silanol and the polymerized functional group other than the group of silanol. Group silanol in such a silane binder compound may enter into a crosslinking reaction with the hydroxy group present on the surface of the inorganic filler by heating or other similar effects, resulting silane binding compound binds to the surface of the inorganic filler that helps to improve the dispersive ability of the pigment in the organic component. Examples of curable functional groups other than the group silanol are a group of acryloyl, a group of methacryloyl, vinyl group, propenyloxy group, butadienyl group, stoilova group, atenolola group, acrylamide group and hydroxy group is A.

In the present invention preferably can be used, for example, silane binder compounds available on the market under the brand names TSL 8350, TSL-8337, TSL-8370, TSL-8375 (all of these materials produces GE Toshiba Silicones), And-9530 (produced by the company Shin-Nakamura Chemical) and a-187 (manufactured Nippon Unicar).

Methods of obtaining inorganic filler treated with a surface does not specifically limited, so this filler can be obtained, for example, in the following way. The above silane binder compound is mixed with an inorganic filler is added to a mixture of ion-exchange water solution and kept for some time at room temperature, passed to the hydrolysis of the silane binder compounds. The time required for hydrolysis depends on the materials used and is usually from 1 hour to 24 hours. After the hydrolysis of the silane binder connection failed sufficiently, the mixture is heated to a temperature of 20°C to 150°C to group silanol in silane binder connection entered into reaction with the hydroxy groups on the surface of the inorganic filler. Thus, it is possible to obtain inorganic filler treated with a surface.

(Other additives)

The alignment layer according to the present invention may also contain, in addition to indicated the data of the above compounds photosensitizers, the equalizer, lubricants, plasticizers, ultraviolet absorbers of radiation, antioxidants, antistatic compounds, pigments, dyes, etc. to the extent that this does not preclude the achievement of the objectives of the invention.

[Method of manufacturing the alignment layer]

The alignment film according to the present invention can be manufactured by applying a liquid coating to create a leveling layer (hereinafter sometimes simply referred to as "liquid coating) on the surface of the transparent polymer base, which must be performed leveling layer, followed by thermal drying and curing.

A method of manufacturing a layer according to the present invention is not restricted to until satisfied the requirements for the content of particles specified by this invention. Next will be described a method of manufacturing a layer is particularly preferable to satisfy the requirements for the content of particles specified by the present invention.

(Liquid coating to create a leveling layer)

Liquid coating to create the alignment layer according to the present invention is a solution obtained by adding a binder polymer resin, an inorganic filler, in some embodiments, the initiator of photopolymerization, and if necessary the value of some other additives in a solvent and subsequent mixing. Each component may be added in solid form, for example in the form of powder or in the form of a solution using a suitable solvent or dispersant. The choice of solvent for use in the composition of the liquid coating does not specifically limited as long as the solvent has satisfactory characteristics from the viewpoint of the solubility of the binder polymer resin and dispersive ability of the pigment, inorganic filler, so you can use the usual organic solvents. For example, it is possible to use ketones, such as methyl ethyl ketone, methyl isobutyl ketone and cyclohexanone, alcohols such as methanol, ethanol, propanol, n-butanol, secondary butanol, t-butanol and isopropyl alcohol, esters such as butyl acetate and ethyl acetate, aromatic hydrocarbons such as toluene and xylene, and glycol esters such as propylene glycol monomethyl ether and propylene glycol monomethyl ether acetate, which increases the dispersive ability of the pigment liquid coatings and to improve the appearance of the alignment layer. In particular, due to the excellent solubility, it is preferable to use ketones and particularly preferable to use methyl ethyl ketone and methyl isobutyl ketone.

The concentration of solids in the liquid coating ranges from 25% to 45% by weight. When the concentration of the solids in the liquid coating is within the specified limits, it is possible to reduce the average diameter and the number of foreign particles on the surface of the alignment layer. When the concentration of solids is too small, the content of the diluting solvent in the liquid coating is too large, resulting in a high probability of violations of the dispersed state of the inorganic filler in the liquid coating, it becomes possible formation of aggregates, which leads to an increase in the average diameter and the number of foreign particles on the surface of the alignment layer. At the same time, when the concentration of solids is too high, the viscosity of the liquid coating is too large, resulting in probable is the formation of gelatinous particles under the influence of the efforts of a shift in the coating process, which leads to an increase in the average diameter and the number of foreign particles on the surface of the alignment layer. From this point of view, the concentration of solids in the liquid coating should be preferably in the range from 30% to 42% by weight and particularly preferably in the range from 35% to 40% by mass.

(The method of applying a liquid coating to create a leveling layer)

According to the present invention for applying liquid coatings to create the alignment layer may be used any known method It may be, for example, the way the guiding edge (lip direct method), a method using a tool in the form of a comma (comma coater method, a method with reversed slit (slit reverse method), a method using a slit die (die coater method, a method with the engraved cylinder (gravure roll coater method, a method using a doctor blade (blade coater method, a sputtering method (spray coater method, a method using an air squeegee (air-knife coating method), a method of dipping (dip coating method) and a method using a rod device (bar coater method). In particular, preferred is a method using an engraved cylinder (gravure coating). According to the present invention is especially preferable to use a method using a reversed engraved cylinder and a method using a reversed engraved cylinder of small diameter (this means, for example, using a device for coating using microgravitational cylinder, manufactured by Yasui Seiki, etc. and the words "small diameter" means a diameter not exceeding 100 mm, preferably not more than 80 mm), which allows to reduce the average diameter and the number of foreign particles on the surface of the alignment layer.

For coating, it is preferable to use the engraved cylinder with a density of lines from 50 to 90 lines per inch. The density of lines here oznachaet the number of recesses, engraved in the surface of the cylinder on the segment of length 1 inch. When using an engraved cylinder with a density of lines in the above limits is possible to reduce the average diameter and the number of foreign particles on the surface of the alignment layer to achieve the standard set by the present invention. When applying liquid coating using an engraved cylinder having a too low density lines, if you want to get above the preferred thickness of the layer, the concentration of the liquid coating becomes too low. Accordingly, for the same reason as in the case of too low concentration of solids in the liquid coating, the average diameter and the number of foreign particles on the surface of the alignment layer increase. At the same time, when applying the liquid coating using an engraved cylinder having a too high density of lines, the shear stress acting on the liquid coating per unit area, increase and become too large, so that it becomes probable the formation of gelatinous particles, resulting in average diameter and the number of foreign particles on the surface of the alignment layer grow. From this point of view is particularly preferably used engraved qi is Indra with the density of lines from 60 to 80 lines/inch.

In addition, according to the present invention it is necessary that the ratio of rotation of the engraved cylinder (the ratio of the speed of rotation of the engraved cylinder (unit: m/min) line speed (the speed of movement of the canvas transparent polymer basis) (unit: m/min) (unit: %) was in the range of 60% to 100%. When the ratio of rotation of the engraved cylinder is in the above range, it is possible to reduce the average diameter and the number of foreign particles on the surface of the alignment layer to the level established by the present invention. If the rate of rotation is too small, increase the exposure time of the shear stresses at the liquid surface, which leads to the increase of the content of foreign particles in the liquid coating, resulting in average diameter and the number of foreign particles on the surface of the alignment layer increase. From this point of view, the ratio of rotation of the engraved cylinder should preferably be in the range of 60% to 80%.

As described above, the liquid coating is applied on a transparent polymer base to create the coating film and then the film coating is dried by heating. With regard to conditions of thermal drying, the film is heated preferably to a temperature of from 50 to 150°C and incubated for from 10 to 150 C, yet b is more preferably heated to a temperature of from 50 to 120°C and aged from 20 to 130 and particularly preferably heated to a temperature of from 50 to 80°C and incubated for from 30 to 120 C. After heat drying the coating film of utverjdayut by ultraviolet radiation or electron beam irradiation. In the case of ultraviolet radiation, the radiation dose is preferably from 10 to 2000 MJ/cm2even more preferably from 50 to 1500 MJ/cm2and particularly preferably from 100 to 1000 MJ/cm2that can further enhance the effect of increasing the hardness of the surface.

Thus, it can be obtained alignment film containing a performed on a transparent polymer base levelling layer satisfying the requirements to the content of the particles according to the present invention.

Examples

Further, the present invention will be described in more detail by examples. To assess the characteristics of the films in these examples used the following methods.

(1) the Thickness of the leveling layer

The alignment film is cut with a sharp blade and examine the resulting cross-section through an optical microscope to measure the thickness of the alignment layer. Measurements are performed at 10 arbitrary points, and take the average value of the measured values as the thickness of the levelling layer (unit: μm).

(2) Measurement of warpage

Of the alignment film cut out a flap size of 10 cm×10 cm and subjected to thermal treatment temperature is round 120°C for 30 minutes Previous heat treatment of the sample is allowed to Mature on the horizontal flat surface of the table so that the curvature was sent bulge down, and measure the height of the edges above the surface of the table. In this way measure the five samples and take the average value of the measurement results as a measure of distortion (unit: mm). During the height of the edges, take the height of the highest portion relative to the surface of the table.

(3) the Average diameter and the number of foreign particles on the surface of the alignment layer

Of the alignment film cut out a flap size of 1 m×1 m At a height of 15 cm above the leveling layer of the composition of the alignment film placed tri-band fluorescent lamp so that the intensity on the surface of the alignment film was not less than 2000 Lux. In such circumstances, looking at the surface of the alignment layer and celebrate visually detected foreign particles. Then marked particles are examined under the microscope and determine the average diameter of particles in the following way. To this end average four sizes such foreign particles - the greatest diameter, the length in the direction perpendicular to the greatest diameter and length in directions at an angle of ±45° to the greatest diameter, and taking the obtained average value as cf is the last of the diameter (unit: μm). Such measurements are performed for all observed particles. Then count the number of detected foreign particles with an average diameter ranging from 20 μm to 100 μm and determine the number of such particles per unit area (units: number of particles/m2).

It is believed that the size of the particles, distinguished by the naked eye, is usually 50 μm or more. However, it was shown that the alignment film according to the present invention due to the effects of optical lenses around foreign particles it was possible to visually identify particles with the real size of about 15 microns.

(4) the Coefficient of defects in thin-film transistor (TFT)

Thin-film transistors formed on the surface of the alignment layer of the composition of the compensating film as described below. Then measured the performance of field-effect transistors with channel p-type (p-channel transistors operating in the mode of enrichment and determined the ratio of the currents in the open and locked position (ON/OFF ratio (the ratio of current flow when the voltage at the drain 40 and the gate voltage minus 50 V and 0 V)) for each transistor. If this ratio (ON/OFF ratio) was not more than 102the device is recognized unusable. The number of unhealthy when the Directors divided by the total number of devices and the resulting ratio was taken as the ratio of defects (unit: %). It is desirable that the coefficient of defects did not exceed 0.1%.

Example 1

<Production of liquid coatings to create easily glue layer>

Polyester: Used polyester material having an acid component containing 65 mole% 2,6-naphthalen dicarboxylic acid/30 mole% isophthalic acid/5% mol of 5-sodium sulfoisophthalic acid, and a glycol component comprising 90 mole% ethylene glycol/10 mole% diethylene glycol (the glass transition temperature Tg=80°C, average molecular weight: 13000).

For producing such a polyester material used in the method described in the patent Application of Japan JP-A-6-116487, Example 1. In other words, was charged to the reactor 100 parts of dimethyl 2,6-naphthalenyloxy, 37 parts of dimethyl isophthalate, 9 parts of dimethyl 5-sodium sulfoisophthalate, 75 parts of ethylene glycol and 6 parts of diethylene glycol and add to 0.05 part of tetramethoxysilane. The mixture is heated and kept in a nitrogen atmosphere at a controlled temperature of 230°C for the implementation of the interesterification reaction, driving away while the formed methanol. After that, the temperature of the reaction system is slowly increased to 255°C and reduced pressure of 1 mm Hg for the implementation of the polycondensation reaction and obtain a polyester.

Using tetrahydrofuran as a solvent obtained in the usual way Polia the IRNA material used in the form of a dispersion in water (concentration of solids: 15% by mass).

Acrylic material: Used acrylic material containing 30 mole% 2-Isopropenyl-2-oxazoline/10 mole% polyethylene oxide (n=10) methacrylate/30 mole% acrylamide (the glass transition temperature Tg=50°C).

For the manufacture of such acrylic material used in the method described in the patent Application of Japan JP-A-63-37167, Technological examples 1-3. In other words, in having four of the neck of the retort download 3 parts lauryl sulfonate sodium as surfactants and 181 part of ion exchange water solution and heated to 60°C in a stream of nitrogen gas. After that, as the polymerization initiators added 0.5 part of ammonium persulfate and 0.2 part of hydronitrate sodium. Later in the retort drip method over 3 hours, add a mixture of 23.3 parts of methyl methacrylate, 22.6 parts of 2-isopropyl-2-oxazoline, 40.7 parts of polyethylene oxide (n=10) methacrylate and 13.3 parts of acrylamide, while maintaining the liquid temperature in the range from 60 to 70°C. After completion of the drop addition of this mixture, soak the material obtained at the above temperature for 2 hours, stirring. Then the system is cooled down and get water acrylic suspension (concentration of solids: 35% by weight).

Additive: Used filler made of silicon oxide (average particle size: 100 nm) (manufactured Nissan Chemica Industries, brand: Snowtex ZL).

Surfactant: Used polyoxyethylene (n=7) lauryl ether (produced by the company Sanyo Chemical Industries, brand: NAROACTY N-70).

The above materials are mixed in the following proportions, calculated on solid matter: 60% polyester, 30% acrylic, 5% additive, 5% surfactant - all percentages by weight. The mixture was thoroughly stirred and diluted with ion exchange water solution until the concentration of solids 8% by weight. Thus, it was made of liquid coating to create easily glue layer.

<the Creation of a transparent polymer base and easily glue layer>

Molten polyethylene terephthalate (viscosity [η]=0.62 DL/g) (dl/g) (25°C, artocarpeae), the glass transition temperature Tg=78°C) produced from the extruder and cooled on the surface of the cooling drum in the usual way to obtain unstretched films. In subsequent this unstretched film is stretched 3.4 times the original length in the longitudinal direction for receiving longitudinally and uniaxially stretched film. Then prepared as described above, the liquid coating to obtain an easily adhesive layer evenly applied with a roller on both sides of the specified longitudinally and uniaxially stretched film. In the future, the film is stretched 3.6 times otnositel the original length in the transverse direction at a temperature of 125°C and conduct heat shrinkage at a temperature of 220°C, preventing the shrinkage of 3% in the width direction to obtain a transparent polymer base thickness of 188 μm with the surface of the easily adhesive layer. The thickness of the easily adhesive layer is 0.04 μm.

<a Liquid coating to create a leveling layer>

The coating material containing as main components a binder polymer resin having as a main component dipentaerythritol hexa(meth)acrylate (refractive index: 1,53), and silicon oxide as the inorganic filler (surface treated celanova binder compound, average particle size: 20 nm, refractive index: 1,47) (produced by the company JSR Corporation, trade name: Z7501 the refractive index after drying: 1,51, the mass ratio of solids binder polymer resin and inorganic filler: 60:40)was diluted with methyl ethyl ketone (MEK) to the concentration of solid matter of 37.5% by weight. In the liquid added silicone oil (produced by the company Shin-Etsu Chemical, trade name: CR-341) as compensation in the amount of 0.12% by weight relative to the solids content in the liquid coating. The resulting liquid coating to create a leveling layer.

<Creating a leveling layer>

The above-described liquid coating to create Firawn the covering layer with use of the device for coating the basis microgravitational cylinder, manufactured by Yasui Seiki (density of lines engraved on the cylinder: 70 lines/inch, diameter: 50 mm), uniformly applied by a reverse engraving on one surface of a transparent polymer base with easy glue layer, so that the film thickness after drying/curing was 6 μm. At this point, the ratio of the speed of rotation of the engraved cylinder to the linear velocity (the ratio of rotation of the engraved cylinder) was set at 70%. Subsequently, after drying for 2 min at 70°C the film was irradiated with ultraviolet light through the device to ultraviolet radiation (the company produces Fusion UV Systems Japan, brand: Fusion H Bulb) when the irradiation intensity of 200 MJ/cm2. Thus was made the alignment film having the alignment layer made on a transparent polymer base.

Table 1 presents the characteristics of the thus created the alignment film and the alignment layer.

<Production of thin-film transistor (TFT)>

Subsequently on the surface of the alignment layer made from the composition described above, the alignment film was considered further by the way made of organic thin-film transistor TFT with located above the shutter. The substrate size of 12 cm×12 cm, and the and it made 500x500 organic thin-film transistors, located within the field size of 10 cm×10 cm substrate (estimated pixel pitch: 200 μm).

1. The creation of the electrodes of the source/drain

On the alignment film by a sputtering method was applied film of copper (position 2 in figure 2) with a thickness of 50 nm, was closed this film commercially available photosensitive resist and dried for formation of the layer of photoresist with a thickness of 2 μm. Then by means of a semiconductor laser with a wavelength of 830 nm and an output power of 100 mW was irradiated to the photoresist at the flux density of energy of 200 MJ/cm2for the display of lines of tracks electrodes and source/drain, and then showed the photoresist aqueous alkaline solution to obtain an image of the resist. Further triggered copper with unnecessary areas by dissolving it in a mixture of dilute sulfuric acid with dilute nitric acid and completely remove the resist by means of an alkaline solution to obtain a picture of electrodes and source/drain (position 4 or 5 in figure 2). The width of these electrodes and source/drain amounted to 40 μm, and the width of lines of tracks was 30 μm.

2. The organic semiconductor layer

On a substrate mounted on a heated up to 60°C hot plate in a nitrogen atmosphere, over performed on this substrate, drawings electrodes drip submitted a solution of pentacene (1,0%) in toluene. As a result, this padlock the formed organic semiconductor layer (pos.6 figure 2) thickness of 200 nm.

3. Creating an insulating layer

First, polystyrene (PS): manufactured by Aldrich Corporation (the average molecular weight Mw=280000 (by way of gel permeation chromatography (GPC))) dissolved in toluene to a concentration of 5% and pass through a filter of 0.45 μm. After this, the solution of polystyrene was applied to the surface of the organic semiconductor layer is performed in stage 2 above, the centrifugal method, the rotation speed of 3000 rpm for 120 seconds and dried in vacuum at 90°C for 30 minutes the result was obtained insulating layer (pos.7 figure 2).

4. The creation of the electrode shutter

When the alignment film is made of insulating layer, etc. on top of this layer through a mask with a given pattern besieged aluminum. As a result, the gate electrode (item 8 in figure 2).

5. Creating a protective layer

Leaving protected by the mask, the contact to the gate electrode, on the surface napisali oxynitride silicon SiOxNyfor formation of a protective layer (position 9 in figure 2).

Features made in this way, the thin-film transistor (TFT) is provided in Table 1.

Example 2

Organic thin-film transistor manufactured in the same way as in Example 1, except that the electrodes of the source/drain were made of gold. In this example, as the liquid provide the Etchant DL the electrodes was used Aqua Regia. In Table. 1 shows the characteristics of the alignment film and the alignment layer, and the obtained thin-film transistor (TFT).

Example 3

The alignment film and thin-film transistor (TFT) is fabricated in the same manner as in Example 1, except that the rate of rotation of the engraved cylinder when manufacturing the alignment layer was set to 100%. Table 1 shows the characteristics of the alignment film, alignment layer, and the obtained thin-film transistor (TFT).

Comparative example 1

The alignment film and thin-film transistor (TFT) is fabricated in the same manner as in Example 1, except that instead of the company's products JSR Corporation trademark: Z7501 was used, the coating material containing the acrylic composition as a binder polymer resin and not containing inorganic filler (produced by the company Dainichiseika Color &Chemicals Mfg., EXF-D202)) (concentration of solids: 70% by mass). Table 1 shows the characteristics of the alignment film, alignment layer, and the obtained thin-film transistor (TFT).

Comparative example 2

The alignment film and thin-film transistor (TFT) is fabricated in the same manner as in Example 1, except that the rate of rotation of the engraved qi is Indra in the manufacture of the alignment layer was set to 40%. Table 1 shows the characteristics of the alignment film, alignment layer, and the obtained thin-film transistor (TFT).

Comparative example 3

The alignment film and thin-film transistor (TFT) is fabricated in the same manner as in Example 1, except that the concentration of solids in the composition of the liquid coating to create a leveling layer was 20% by weight. Table 1 shows the characteristics of the alignment film, alignment layer, and the obtained thin-film transistor (TFT).

These results show that only when the requirements of the present invention thin-film transistor (TFT)made directly on the leveling layer, have a low coefficient of defects.

Table 1
Conditions causingThe alignment filmThin-film transistor
Levelling layer
The concentration of solids in the liquid coating to create a leveling layer The ratio of rotation of the engraved cylinderThicknessThe number of foreign particles with a mean diameter of 20-100 μmWarpingThe factor of defects
Unitsweight%%mcmthe number of particles/m2mm%
Example 137.57062100.03
Example 237.57062100.05
Example 337.51008.55200.06
Comparative example 137.5706 10100.5
Comparative example 237.54041650.7
Comparative example 3207032031.0

The advantages of the present invention

The present invention makes possible the creation of the alignment film with a reduced number of defects. In addition, the present invention makes possible the creation of the alignment film, which when used for the substrate in the thin-film transistor (TFT) can significantly reduce the number of defective transistors, even if such a thin-film transistor is formed directly on the film, and thereby prevents the formation of line defects. Thus, the alignment film according to the present invention is particularly suitable for substrates in thin film transistors (TFT).

Applicability in industry.

The alignment film according to the present invention differs reduced quantities of the m particles of a certain average diameter and contains fewer defects with excellent flatness. As a result, when using such alignment film of the substrate in the thin-film transistor (TFT) even when the creation of such a transistor directly on the film can sufficiently reduce the formation of defective transistors. In addition, you can accordingly reduce the probability of formation of linear defects. Thus, the alignment film according to the present invention is particularly suitable for substrates in thin film transistors. In particular, such a leveling film can be used for creating various thin-film transistors, such as organic thin-film transistors, transistors made of amorphous silicon and transistors from crystalline silicon and thin-film devices, a variety of displays, field emission, electroluminescent (EL) displays, liquid crystal displays, electrochromic devices, etc.

1. The alignment film for the substrate in the thin film transistor containing alignment layer including a binder polymer resin and the inorganic filler as component, at least one side of a transparent polymer base,
the number of foreign particles with a mean diameter of from 20 μm to 100 μm on the surface of leveling the layer does not exceed 5/m 2.

2. The alignment film according to claim 1, in which the leveling layer has a thickness in the range from 3 μm to 8 μm.

3. A method of manufacturing the alignment film according to claim 1, containing a stage of applying a liquid coating on a transparent polymer base for forming the alignment layer, in which liquid coating obtained by adding at least a binder polymer resin and the inorganic filler in the solvent and subsequent mixing
the concentration of solids in the liquid coating is in the range from 25% to 45% by weight, and the liquid coating is applied using an engraved cylinder, having a density of lines 50-90 lines/inch, at a rate of rotation from 60% to 100%, and then dried/utverjdayut for the formation of the alignment layer.



 

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1 ex, 1 tbl

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Infrared reflector // 2510055

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5 cl, 2 tbl, 14 ex

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11 cl, 5 dwg, 8 tbl

FIELD: chemistry.

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3 dwg, 3 tbl

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SUBSTANCE: composition for spraying a fluoropolymer on a polyimide film is an aqueous dispersion of a fluoropolymer to which a 50% water-alcohol solution is added in ratio of 1:1. The device for depositing a fluoroplastic coating on the surface of a polyimide film has a supporting drum with a heated outer surface which is equipped with a drive which determines the rotational speed of the drum, which provides given tension in the polyimide film. The unit for spraying the fluoropolymer dispersion onto the surface of the polyimide film has a sprayer which moves across the polyimide film.

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7 cl, 1 dwg

FIELD: process engineering.

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EFFECT: higher wear resistance and surface hardness.

3 cl, 1 tbl, 10 ex

FIELD: chemistry.

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3 cl, 4 dwg, 3 tbl

FIELD: process engineering.

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17 cl, 2 dwg, 4 tbl

FIELD: chemistry.

SUBSTANCE: claimed invention relates to suitable for smoking and jerking single-layered or multi-layered sleeve food film, in particular to sausage casing for smoked and/or jerked sausage or meat products, and to method of its manufacturing. Said food film is manufactured from homogeneous melted polymer material on installation for (combined) extrusion of food film by formation with blowing by means of supply (jointly) of polymers to be extruded to nozzle of blow head and biaxial orientation in the process of triple blowing. Homogeneous polymer melt of polymers for film manufacturing represents mixture of polymers, consisting of: polyethylene terephthalate or mixture of different polyethylene terephthalates and polyvinyl alcohol, or polyethylene terephthalate or mixture of different polyethylene terephthalates and block-copolymer of polyether with amides, or polyethylene terephthalate or mixture of different polyethylene terephthalates, polyvinyl alcohol and block-copolymer of polyether with amides.

EFFECT: claimed food film provides such fey parameters as suitability for smoking, which is determined by permeability for oxygen and water vapour, as well as adsorption of oxygen and water vapour, colouring surface of filled product, rigidity and strength.

18 cl

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