KR101463472B1 - Pressure control members and method for manufacturing the same, pressure control unit and vacuum deposistion apparatus containing the same - Google Patents

Abstract

Provided in the present invention are a pressure control member which controls pressure by being installed on such a vacuum chamber, includes ceramic particles having average particle size of 1-50 μm; and an inorganic binder binding the ceramic particles, and has porosity of 25-40%, and a method for manufacturing the same. Moreover, provided in the present invention are a pressure control unit and a vacuum deposition apparatus including the pressure control member. According to the present invention, if the vacuum state is broken, generation of vortex caused by extreme pressure change is prevented or minimized to effectively prevent contamination of such a thin film.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a pressure regulating member, a pressure regulating member, a pressure regulating unit, and a vacuum deposition apparatus including the pressure regulating member,

The present invention relates to an apparatus for maintaining a vacuum of atmospheric pressure or lower, for example, a pressure regulating member installed in a vacuum deposition chamber or the like to regulate pressure, a method of manufacturing the same, and a pressure regulating unit including the pressure regulating member, ≪ / RTI >

Generally, electric and electronic devices (devices) and optical devices include electrodes and dielectrics, and most of these electrodes and dielectrics are composed of thin films. The thin film is formed by depositing a metal or a metal oxide. At this time, in the case of a conductive thin film (electrode), a metal oxide thin film such as a two-component system or a three-component system is mainly used. As the conductive thin film, for example, a transparent thin film such as indium-tin oxide (ITO), aluminum-zinc oxide (AZO) and indium-gallium-zinc oxide (IGZO) is used. As the dielectric thin film (dielectric), ABO-based oxides are mainly used. Specific examples thereof include Pb (Zr _x Ti _{1 -x} ) O ₃ or (Ba _x Sr _{1 -x} ) TiO ₃ Oxide thin films are used.

In forming the thin film as described above, physical vapor deposition (PVD), chemical vapor deposition (CVD), and a deposition method in which these are combined are used. In order to realize deposition, a vacuum deposition apparatus is usefully used. For example, in Korean Patent Laid-Open Nos. 10-2001-0098215, 10-2013-0113302, 10-2010-0093495, and 2005-256112, A vacuum evaporation apparatus is disclosed.

At this time, most vacuum deposition apparatuses include a vacuum deposition chamber that maintains vacuum at atmospheric pressure (760 Torr) or less. Specifically, for example, a vacuum deposition apparatus includes a vacuum deposition chamber; A substrate holder installed inside the chamber and to which the substrate is fixed; And a sputter gun installed inside the chamber and on which a target is mounted. The vacuum deposition apparatus may also include, for example, a shutter assembly or the like for preventing contamination of the target, in addition to the above-described components.

A cathode is mounted on the sputter gun. The target is composed of a thin film raw material. The target is composed of a metal oxide as specifically described above, but mostly composed of a powder-bulk type. In addition, the vacuum deposition chamber is provided with an exhaust port for forming a vacuum and a gas inlet for breaking a vacuum. At this time, a vacuum pumping system is connected to the exhaust port to form a vacuum in the chamber. After deposition, the gas is injected into the gas injection port to destroy the vacuum.

However, most vacuum deposition apparatuses according to the prior art generate plasma by injecting argon, argon, oxygen, or other gas as a source of the plasma required for vacuum deposition. In the prior art, the plasma generating gas is unevenly distributed, and the quality of the deposited film deteriorates when the vacuum degree of the deposition varies due to the discharge of gas generated during deposition. Further, there is a problem that contamination occurs in a thin film or the like due to an extreme pressure change when the vacuum is destroyed. Specifically, in a vacuum deposition chamber maintained at a low pressure vacuum (for example, a pressure of 1 Torr or less), fine particles generated by deposition together with a gas containing a high temperature deposition starting material (for example, metal oxide particles ). At this time, eddy flow is generated in the chamber due to extreme pressure change (for example, 1 Torr -> 760 Torr) in the process of breaking the vacuum through the injection of gas into the gas injection port. Such a vortex causes a problem that the fine particles adhere to the surface of the thin film (product) to cause contamination. If the fine particles are contaminated with such a material, the quality of the thin film is deteriorated. For example, in the case of a conductive thin film, the resistance can be increased.

Published Patent No. 10-2001-0098215 Patent Publication No. 10-2013-0113302 Published Patent No. 10-2010-0093495 Japanese Patent Laid-Open No. 2005-256112

Accordingly, it is an object of the present invention to prevent abrupt change in working vacuum during deposition and to prevent or minimize occurrence of vapors in vacuum evacuation, for example, to effectively maintain the quality of a thin film and to prevent contamination of thin films due to abrupt changes in working vacuum degree And a pressure regulating unit including the pressure regulating member and a vacuum deposition apparatus.

It is another object of the present invention to provide a method of manufacturing a pressure regulating member capable of manufacturing a pressure regulating member in an efficient process even in a short time while having excellent mechanical strength and the like.

The pressure regulating member according to the present invention comprises ceramic particles having an average particle size of 1 to 50 μm; And an inorganic binder for binding the ceramic particles, and has a porosity of 25% to 40%.

At this time, the pressure regulating member according to the present invention preferably has a density of, for example, 1.4 g / cm3 to 1.6 g / cm3.

Also, a method of manufacturing a pressure regulating member according to the present invention is a method of manufacturing a pressure regulating member, comprising: a first step of obtaining a mixture containing ceramic particles having an average particle size of 1 to 50 μm, an inorganic binder for bonding the ceramic particles, step; A second step of drying the mixture; A third step of compression molding the dried mixture to obtain a molded body; And a fourth step of baking the molded body.

The pressure regulating unit according to the present invention may further include: the pressure regulating member; And a glass or quartz connection pipe coupled to the end of the pressure regulating member.

In addition, a vacuum deposition apparatus according to the present invention includes: a vacuum deposition chamber in which a gas injection port is formed; And a pressure regulating member or a pressure regulating unit provided in the gas inlet.

According to the present invention, it is possible to prevent or minimize the occurrence of eddy currents caused by extreme pressure changes, thereby effectively preventing contamination of evaporated products such as thin films.

Further, according to the present invention, it is possible to efficiently manufacture the pressure regulating member even in a short time while having excellent mechanical strength and the like.

1 is a photograph of a pressure regulating member manufactured according to an embodiment of the present invention,
2 is a SEM photograph of the surface of the pressure regulating member manufactured according to the embodiment of the present invention,
FIG. 3 is a graph showing density measurement results according to molding pressures of pressure control members manufactured according to Examples and Comparative Examples of the present invention,
4 is a view showing an example of a pressure control unit according to the present invention, which is a photograph showing a quartz tube coupled to the pressure regulating member of FIG. 1, and FIG.
5 is a schematic view of a vacuum deposition chamber using a pressure regulating member according to an embodiment of the present invention.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. Prior to this, terms and words used in the present specification and claims should not be construed as limited to ordinary or dictionary terms, and the inventor should appropriately interpret the concepts of the terms appropriately It should be construed in accordance with the meaning and concept consistent with the technical idea of the present invention based on the principle that it can be defined. It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory and are not intended to limit the invention to the particular embodiments, It is to be understood that the invention includes all modifications, equivalents, and alternatives falling within the scope. It should also be understood that various equivalents and modifications may be substituted for those at the time of the present application.

Hereinafter, the present invention will be described in detail.

The present invention provides a pressure regulating member capable of regulating pressure and a preferable method for producing the same. The present invention also provides a pressure control unit and a vacuum deposition apparatus including the pressure regulating member.

The pressure regulating member according to the present invention is used, for example, in an apparatus for maintaining a vacuum below atmospheric pressure, specifically in a vacuum chamber or the like, for regulating the pressure in the chamber. In the present invention, the term 'pressure control' may be used, for example, to prevent extreme pressure changes in the chamber, minimize the occurrence of vortexes, or preferably completely prevent the occurrence of vortexes.

The pressure regulating member according to the present invention can be usefully used for pressure regulating, for example, controlling a vacuum of 760 Torr or less, more specifically, a vacuum of 0 to 50 Torr, to a pressure of atmospheric pressure (760 Torr) or more. That is, the pressure regulating member according to the present invention can be advantageously used for the purpose of vacuum breaking members capable of breaking a vacuum.

Further, the pressure regulating member according to the present invention can be used, for example, in a gas injection port of a vapor deposition facility to regulate the pressure of gas. For example, it can be applied to a gas nozzle for plasma generation in a vapor deposition system such as physical vapor deposition (PVD) or chemical vapor deposition (CVD). At this time, the pressure regulating member according to the present invention distributes the plasma generating gas evenly in the chamber, thereby achieving a low change in the internal working vacuum degree. Particularly, when applied to a large chamber, the rate of change of the vacuum degree distribution inside the chamber is kept low.

The pressure regulating member according to the present invention is installed, for example, in a gas inlet for vacuum evacuation of a vacuum deposition chamber to regulate the gas pressure during vacuum evacuation. That is, at the time of injecting gas for vacuum evacuation, extreme pressure change due to gas injection is prevented, and vortex generation is prevented. This prevents contamination of the vapor deposition product (thin film, etc.) by the eddy current. In the following description of the present invention, the pressure regulating member according to the present invention will be described as an example of a vacuum cleaner.

The pressure regulating member according to the present invention is a porous ceramic material comprising ceramic particles and an inorganic binder for binding the ceramic particles. At this time, the ceramic particles are bonded to each other by an inorganic binder through high-temperature firing. A plurality of pores are formed between the ceramic particles. The pressure regulating member according to the present invention has a porosity of 25% to 40%. In the present invention, the porosity means the volume percentage (%) occupied by pores in the entire volume of the pressure regulating member according to the present invention. The porosity is specifically expressed by the following equation.

Porosity (%) = (Vp / V) x 100

Here, V is the total volume of the pressure regulating member, and Vp is the total volume of the pores formed in the pressure regulating member.

In the present invention, the porosity acts as an important factor in controlling the pressure. At this time, if the porosity is less than 25%, it may be effective to prevent extreme pressure change, but the time required for vacuum digging may be too long. If the porosity exceeds 40%, the pressure change is too severe to generate a vortex in the chamber, and thus contamination may occur. Considering this point, it is preferable that the porosity is 30% to 35%. The porosity can be controlled, for example, by controlling the size of the ceramic particles, the content of the resin binder and / or the molding pressure as described later.

Further, the ceramic particles are selected from those having an average particle size of 1 to 50 mu m. The size distribution of these ceramic particles affects porosity and mechanical strength. Specifically, when the average size of the ceramic particles is less than 1 占 퐉, the porosity becomes too low and the vacuum purging time may become longer. When the average size of the ceramic particles exceeds 50 탆, the porosity becomes too high and a vortex may be generated at the time of evacuation of the vacuum, which may also reduce the mechanical strength and the like. Considering this point, it is preferable that the ceramic particles have an average particle size of 10 to 50 mu m, more preferably 10 to 40 mu m. In the present invention, 'average particle size' means the average size of the entire ceramic particles used.

The pressure regulating member according to the present invention can be manufactured by various methods as long as it can be produced to have a porosity of 25% to 40% by using ceramic particles and an inorganic binder as main materials, and the manufacturing method thereof is not particularly limited Do not. According to a preferred form, the pressure regulating member according to the present invention can be manufactured through the method described below.

Hereinafter, a method of manufacturing a pressure regulating member according to the present invention (hereinafter referred to as a "manufacturing method") will be described, and a specific embodiment of the pressure regulating member according to the present invention will be described.

The manufacturing method according to the present invention includes a first step of obtaining a mixture containing ceramic particles, an inorganic binder and an organic material, a second step of drying the mixture, a third step of compression-molding the dried mixture to obtain a molded article, And a fourth step of baking the molded body. And each step is continuous. That is, the manufacturing method according to the present invention includes a step of mixing the raw materials-> the drying step-> the molding step-> the sintering step.

The ceramic particles are selected from those having an average particle size of 1 to 50 탆 in consideration of porosity and mechanical strength of the pressure regulating member as described above. Preferably an average particle size of 10 to 50 mu m, more preferably an average particle size of 10 to 40 mu m.

The kind of the ceramic particles is not particularly limited. The ceramic particles may be selected from inorganic materials containing at least one or more metal elements in the molecule. The ceramic particles preferably include at least one selected from among silica (SiO ₂ ), alumina (Al ₂ O ₃ ), and titania (TiO ₂ ) in consideration of heat resistance and mechanical strength. The ceramic particles, may be preferably comprises at least a silica (SiO _2). Specifically, silica (SiO ₂ ) alone can be used as the ceramic particles. In addition, the ceramic particles may be a mixture of silica and other inorganic materials (SiO _2). In the present invention, silica (SiO ₂₎ include fumed silica (fumed silica).

The inorganic binder is not particularly limited as long as it can bond the ceramic particles by firing. The inorganic binder can be selected, for example, from those which can have melt adhesion upon firing. At this time, in the present invention, the inorganic binder does not mean only inorganic substances but includes inorganic-organic complexes.

According to an exemplary embodiment of the present invention, the inorganic binder preferably includes a silicate. This, in particular, are useful in the present invention in the case where the ceramic particles comprising at least a silica (SiO _2). That is, the silicate is advantageous for improving the bonding force of the silica (SiO ₂ ) particles. At this time, the silicate is preferably selected from ethyl silicate. The silicate preferably contains at least tetraethyl orthosilicate (TEOS) among ethyl silicates. Such tetraethylorthosilicate (TEOS) is coated on the surface of silica (SiO ₂ ) particles during sintering to greatly increase the sinterability of the silica particles, so that excellent bonding force between the silica particles is achieved after firing.

The inorganic binder is not particularly limited, but may be used in an amount of 0.5 to 15 parts by weight based on 100 parts by weight of the ceramic particles. At this time, if the content of the inorganic binder is less than 0.5 parts by weight, the bonding force between the ceramic particles may be weakened. If the content of the inorganic binder is more than 15 parts by weight, the bonding strength may be insufficient due to excessive use, and the amount of the ceramic particles and the organic material may be relatively low, so that it may be difficult to exhibit a good porosity. In consideration of this, the inorganic binder may be used in an amount of 1.0 to 12 parts by weight based on 100 parts by weight of the ceramic particles.

The organic material is used for pore formation. That is, the pressure regulating member according to the present invention has a plurality of pores formed by the elimination of the organic substances at the time of firing to have porosity. The organic material may also function as a shape-retaining function depending on circumstances. More specifically, in the case where the organic material to be used has adhesiveness, for example, the organic material may have a function of bonding the ceramic particles and the inorganic binder to maintain the shape of the preform before molding.

The organic material may be one that can be exhausted by firing to form a large number of pores. The organic material may be selected from, for example, a resin, and the kind thereof is not particularly limited. The organic material specifically includes at least one selected from a thermoplastic resin and a thermosetting resin. The organic material is selected from, for example, polyvinyl alcohol (PVA), polyvinyl butyral (PVB), polyvinyl pyrrolidone (PVP), acrylic resin, urethane resin, epoxy resin, phenol resin and unsaturated polyester resin And may include one or more.

The organic material is not particularly limited, but may be used in an amount of 0.8 to 15 parts by weight based on 100 parts by weight of the ceramic particles. At this time, it may vary depending on the molding pressure applied at the time of compression molding. However, when the content of the organic material is less than 0.8 part by weight, the porosity may be too low. On the other hand, when the content is more than 15 parts by weight, the porosity may be too high. Considering this point, the organic material is preferably used in an amount of 1.2 to 12 parts by weight based on 100 parts by weight of the ceramic particles.

In the first step (mixing), a mixture containing the ceramic particles, the inorganic binder and the organic material is obtained. At this time, a solvent or the like for viscosity control and / or dispersion may be further added to the mixture. The solvent is not particularly limited as long as it can control the viscosity of the mixture and / or improve the dispersibility of the ceramic particles (and inorganic binder) in the mixture. The solvent may be selected depending on, for example, the type of the organic material, and specific examples include water, an organic solvent, and a mixture thereof. Examples of the organic solvent include alcohols such as methyl alcohol, ethyl alcohol, propyl alcohol and butyl alcohol; Ketones such as methyl ethyl ketone (MEK); And aromatic hydrocarbons such as benzene and toluene. In addition, the solvent may be appropriately adjusted within a range of 5 to 300 parts by weight based on 100 parts by weight of the ceramic particles.

Further, according to an exemplary aspect of the present invention, the first step (mixing) may include a secondary mixing step. Specifically, a first mixing step of mixing ceramic particles, an inorganic binder and a solvent (alcohol or the like) first, and a mixing step of adding an organic material (thermoplastic resin and / or thermosetting resin) to the mixture obtained through the first mixing And a secondary mixing process. Thus, when proceeding to the secondary mixing step, for example, the dispersibility of the constituent components can be improved.

In the second step (drying), the mixture thus obtained is dried. In the present invention, the drying may be carried out in such a manner that the mixture can be dried in a powder form capable of compression molding. The drying method is not limited. Drying includes, for example, natural drying, hot air drying and heat drying. In addition, the drying can be carried out at a temperature of, for example, 80 ° C to 100 ° C. Through this drying, a powdery mixture suitable for compression molding is obtained.

In the third step (compression molding), the dried mixture, that is, the powdery mixture is compression-molded to obtain a molded body having a predetermined shape. More specifically, the dried mixture is uniaxially pressed. The shape of the molded body is almost the same as that of the sintered body after firing, that is, the shape of the pressure adjusting member according to the present invention. At this time, the shape of the molded body is not limited. That is, the shape of the pressure regulating member according to the present invention is not limited.

The shape of the molded body (i.e., the shape of the pressure regulating member) may have various cross sectional shapes such as circular, elliptical, or polygonal (e.g., rectangular, hexagonal, octagonal). The shape of the molded body (i.e., the shape of the pressure regulating member) may have a circular cross-sectional shape, for example. In the present invention, a prototype does not mean a complete prototype. The shape of the molded body (i.e., the shape of the pressure regulating member) may have a cylindrical bar shape according to an exemplary embodiment. The molded body (i.e., the pressure regulating member) may be hollow, for example, along the longitudinal direction at the center.

BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 is a photograph of a pressure regulating member manufactured in accordance with an exemplary embodiment of the present invention. As shown in FIG. 1, the pressure regulating member according to the present invention may have a cylindrical shape, for example, with a hollow formed along its longitudinal direction.

The compression molding can be implemented by, for example, a die press or an extruder. At this time, the pressure applied during compression acts as an important factor in the porosity and density of the pressure regulating member. According to a preferred embodiment, it is preferable that the dried mixture is compression molded at a pressure of 1.5 MPa to 20 MPa. At this time, when the molding pressure is less than 1.5 MPa, the porosity may become too large, and the density may be lowered and the mechanical strength may be weakened. If the molding pressure exceeds 20 MPa, the porosity may be too low.

In the fourth step (firing), the compression-molded body is fired (heat-treated). By this firing, the organic particles are exhausted and pores are formed, and the ceramic particles are sintered and bonded via the inorganic binder. At this time, the firing temperature is not limited. The firing temperature may be a temperature capable of sintering the ceramic particles while exhausting the organic matter.

The firing temperature may vary depending on the kind of the ceramic particles and the organic material, but may be 1,000 ° C or higher, for example, 1,000 ° C to 1,500 ° C for good sinterability. At this time, if the firing temperature is less than 1,000 ° C, the sintering property may be slightly small. If the firing temperature exceeds 1,500 ° C, for example, the porosity may be lowered due to the densification of the sintered body. Considering this point, the firing temperature may be preferably from 1,200 to 1,300 ° C.

The firing time is not particularly limited, but may be, for example, 2 hours or more, and for example, 2 hours to 24 hours. The firing time may be more specifically, for example, 5 hours to 15 hours, but it may vary depending on the firing temperature and the like.

The manufacturing method according to the present invention described above facilitates the manufacture of the pressure regulating member according to the present invention. Specifically, as the porous ceramic material, the pressure adjusting member according to the present invention having a porosity of 25% to 40% and excellent mechanical strength can be easily manufactured.

In the production of the pressure regulating member according to the present invention, for example, a method of producing by a wet gel method or a casting method may be considered. However, this method takes a long time and the mechanical strength after firing is low. And it is difficult to control the porosity. On the other hand, when the above-mentioned production method of the present invention, that is, molding by compression after mixing and drying, and then firing, the process time can be remarkably shortened, and also excellent mechanical strength is obtained after firing. Further, as described above, the porosity can be easily controlled by controlling the molding pressure. In addition, the pressure regulating member has a good surface state by compression molding.

In the present invention, the porosity can be controlled by controlling the molding pressure as described above, and can also be controlled depending on factors such as the size of the ceramic particles and the content of the organic matter, as mentioned above. Also, in accordance with an exemplary form of the invention, it may be desirable to have an appropriate density through adjustment of such factors as described above.

At this time, it is preferable that the pressure regulating member according to the present invention has a density of, for example, 1.4 g / cm 3 to 1.6 g / cm 3 through controlling the molding pressure, the size of the ceramic particles and the content of the organic matter. In this density range, excellent porosity can be secured while having excellent mechanical strength. Specifically, when the density is less than 1.4 g / cm 3, it may be difficult to have excellent mechanical strength, and when the density is more than 1.6 g / cm 3, the porosity may be somewhat low.

The pressure regulating member according to the present invention may have a gas passing pressure of 0.5 to 2 kg / cm 2, for example, by controlling the molding pressure, the size of the ceramic particles and the content of the organic matter. When the gas passing pressure is within this range, it is possible to effectively break the vacuum and prevent the occurrence of vortex. Preferably, it may have a gas passage pressure of 0.9 to 1.5 kg / cm 2.

According to a preferred embodiment, the pressure regulating member according to the present invention preferably has a porosity of 30% to 35%, a density of 1.4 g / cm3 to 1.6 g / cm3, and a gas passing pressure of 0.9 to 1.5 kg / . When all of these three conditions are satisfied, the vacuum evacuation can be effectively achieved while having excellent characteristics in preventing vortex generation and mechanical strength.

Meanwhile, the pressure control unit according to the present invention includes the pressure control member of the present invention and at least one connection pipe as described above. At this time, the connection pipe is coupled to at least one end of the pressure regulating member. That is, the connector can be coupled to either end of the pressure regulating member, or to both ends.

Various methods may be considered for coupling the pressure regulating member and the coupling pipe. The connection between the pressure regulating member and the connection pipe may be selected from, for example, fusion bonding, adhesion by an inorganic adhesive, and / or fastening by a separate fastener, but is not limited thereto.

FIG. 4 shows an example of a pressure control unit according to the present invention. 4 is a photograph showing a connection pipe connected to a pressure regulating member manufactured according to an embodiment of the present invention. In Figure 4, the transparent tube is a connector.

The connection pipe may be connected to a gas inlet such as a vacuum deposition chamber, or may be used to connect the pressure regulating member to another external device. Such a connection pipe may be any one capable of fluid flow. The connector may be transparent or opaque, which may also have the same cross-sectional shape as, for example, the pressure regulating member. In addition, the connection pipe may have a curved shape such as an "a" shape, for example, as shown in Fig. 4, in order to change the flow channel as occasion demands. Such connectors can be selected, for example, from glass or quartz materials.

The pressure regulating unit according to the present invention is the same as the pressure regulating member of the present invention as described above in its use. For example, it may be installed in an apparatus for maintaining a vacuum of atmospheric pressure or lower, for example, in a vacuum chamber, and used for purifying vacuum. In addition, the pressure regulating unit according to the present invention can be applied to a gas nozzle for plasma generation, for example, in a vapor deposition apparatus such as physical vapor deposition (PVD) or chemical vapor deposition (CVD).

In addition, the vacuum deposition apparatus according to the present invention includes at least one pressure control member or pressure control unit according to the present invention including a vacuum deposition chamber as described above. The vacuum deposition chamber is formed with at least one gas inlet, which can be selected from conventional ones. At this time, in the present invention, the gas injection port may be at least one selected from a gas injection port for vacuum evacuation and a gas injection port for plasma generation. A pressure regulating member or a pressure regulating unit according to the present invention is installed in the gas inlet so as to break the vacuum or to inject the plasma generating gas at low speed.

The vacuum deposition apparatus according to the present invention may include any one of the above-described vacuum deposition chamber, the pressure regulating member, or the pressure regulating unit. And may include components such as a substrate holder for holding the substrate, a deposition device for depositing and depositing the target, and a shutter assembly for preventing contamination of the target, which are usually provided in the vacuum deposition chamber. The structure and the shape of such components are not limited, and this can be the same as usual.

In the present invention, the evaporator may comprise a deposition element capable of implementing physical vapor deposition (PVD), chemical vapor deposition (CVD), and a combination thereof. The deposition apparatus may have a structure and a shape that can be deposited by a method such as DC sputtering, RF sputtering, magnetron sputtering, reactive sputtering, and electron-beam vapor deposition. The evaporator may include a sputter gun with a cathode, for example.

According to the present invention described above, occurrence of vortex due to extreme pressure changes can be prevented or minimized. This can, for example, prevent contamination of deposited products, such as thin films, in the interior of the chamber during vacuum evacuation, thereby improving the quality of the product.

Further, in the case of the production method according to the present invention, the time for producing the pressure regulating member can be shortened and excellent mechanical strength can be achieved as described above. In addition, the porosity can be easily controlled and the surface property of the pressure regulating member is improved.

Hereinafter, examples and comparative examples of the present invention will be exemplified. The following embodiments are provided to facilitate understanding of the present invention, and thus the technical scope of the present invention is not limited thereto.

[Example 1]

Fumed silica (SiO ₂ ) having a particle size distribution of 10 to 50 μm was prepared. The silica (SiO ₂₎ (isopropyl alcohol aqueous solution of 30wt%) aqueous solution of alcohol relative to 100 parts by weight was stirred and mixed 50 parts by weight of tetraethyl silicate addition (TEOS) 5 parts by weight. Thereafter, 10 parts by weight of polyvinyl alcohol (PVA) was further added, mixed and stirred, and then dried at a temperature of about 90 캜 to obtain a powdery mixture.

Next, the dried powdery mixture was put into a metal mold and subjected to compression molding at a pressure of 1.5 MPa to obtain a hollow cylindrical shaped article. Thereafter, the formed body was put in a sintering furnace and then fired (heat-treated) at a temperature of 1250 ° C. for 10 hours to manufacture a pressure regulating member of the porous ceramic material according to the present embodiment.

[Examples 2 to 5]

In the same manner as in Example 1, molding pressure was varied according to each example during compression molding. (Example 2), 2.5 MPa (Example 3), 5 MPa (Example 4), and 20 MPa (Example 5) according to each of the Examples, . Thereafter, firing was carried out under the same conditions as in Example 1.

FIG. 1 is a photograph of a pressure regulating member manufactured according to Example 3 (molding pressure: 2.5 MPa). 2 is a SEM photograph of the surface of the pressure regulating member manufactured according to Example 3 (molding pressure: 2.5 MPa).

[Comparative Example 1]

Compared with Example 1, the pressure was greatly increased during the compression molding. Specifically, the dried powdery mixture was poured into a mold and pressed, but the molding pressure was increased to 50 MPa. Hereinafter, the firing conditions are the same as in the first embodiment.

The density (g / cm 3) and porosity (%) of the pressure regulating member according to Examples 1 to 5 and Comparative Example 1 were measured, and the results are shown in Table 1 below. 3 is a graph showing density and porosity measurement results according to molding pressure.

Remarks Molding pressure [MPa] Density [g / cm3] Porosity [%] Example 1 1.5 1.37 38 Example 2 2 1.52 31 Example 3 2.5 1.53 30 Example 4 5 1.57 29 Example 5 20 1.66 25 Comparative Example 1 50 1.84 16

As shown in Table 1 and attached FIG. 3, it can be seen that the density and the porosity are changed according to the molding pressure. In other words, it can be seen that the density and the porosity can be controlled by controlling the molding pressure in the compression molding.

[Examples 6 to 8]

The same procedure as in Example 3 was carried out except that silica (SiO ₂ ) particles were different in size. Specifically, the particle size distribution less than 30㎛ (Example 6), particle size distribution 30 ~ 40㎛ (Example 7), and particle size distribution as being 40 ~ 50㎛ (Example 8), silica (SiO ₂ for each Example ) Having different particle size distributions were used. The molding pressure and the sintering conditions were the same as in Example 3.

[Comparative Examples 2 to 3]

As compared with Example 3, silica (SiO ₂ ) having a large particle size distribution was used. Specifically, in the case of Comparative Example 2, silica (SiO ₂ ) having a particle size distribution of 50 to 60 μm was used, and in Comparative Example 3, silica (SiO ₂ ) having a particle size exceeding 60 μm was used . The molding pressure and the sintering conditions were the same as in Example 3.

The density (g / cm 3), the porosity (%) and the gas passing pressure (kg / cm 2) were measured for the pressure regulating members according to Examples 6 to 8 and Comparative Examples 2 to 3, Respectively. In this case, the measurement results of the pressure regulating member according to the third embodiment are also shown in [Table 2].

<Measurement results of physical properties according to the particle size of SiO ₂ > Remarks SiO ₂ Particle Size [탆] Density [g / cm3] Porosity [%] Gas passing pressure [kg / ㎠] Example 3 10 to 50 1.53 30 1.5 Example 6 <30 1.53 31 1.3 Example 7 30 to 40 1.49 33 1.1 Example 8 40 to 50 1.46 34 1.0 Comparative Example 2 50 to 60 1.42 35 0.8 Comparative Example 3 > 60 1.43 36 0.7

As shown in Table 2, the density, porosity and gas permeation pressure are changed depending on the particle size of silica (SiO ₂ ). In other words, it can be seen that, by controlling the particle size of the silica (SiO ₂ ), the density and the porosity as well as the gas passage pressure can be controlled.

For the pressure regulating member according to the above embodiments and comparative examples, the time required for vacuum digging and the degree of contamination of the thin film surface when vapors in the chamber were generated were evaluated as follows.

In this case, the quartz tube is bonded to the end of the pressure control member according to each of the embodiments and the comparative examples (see FIG. 4), and then the vacuum evaporation apparatus is used for vapor deposition of the transparent conductive oxide thin film (electrode) And this was packed into a gas inlet for vacuum evacuation of a vacuum deposition chamber having a volume of 0.2 m 3. Then, the time (seconds) at which the vacuum reached 760 Torr from the initial 1 Torr was measured. After vacuum evacuation, the thin film was observed to evaluate the degree of contamination by the fine particles. At this time, the pollution was evaluated as 10 points, 10 points according to the degree of pollution, 0 point if there was no pollution, 10 points when the pollution was higher, > 0 (none)] The above results are shown in [Table 3]. At this time, in the results of [Table 3], Comparative Example 4 is a result of the specimen in which the pressure regulating member is not provided in the vacuum deposition chamber.

     &Lt; Evaluation results of vacuum breakage time and pollution degree > Remarks The pressure-
Installation Yes / No SiO ₂ Particle Size
[Mu m] Porosity
[%] Vacuum destruction time
(1 Torr -> 760 Torr)
[sec] Degree of pollution Example 3 U 10 to 50 30 300-320 0 Example 6 U <30 31 290-310 0 Example 7 U 30 to 40 33 260-280 0 Example 8 U 40 to 50 34 220 ~ 240 0 Comparative Example 1 U 10 to 50 16 460-480 One Comparative Example 2 U 50 to 60 35 180 ~ 200 2 Comparative Example 3 U > 60 36 140-160 3 Comparative Example 4 radish - - 50 to 60 10

As shown in [Table 3], it can be seen that the time required for vacuum digging and the degree of contamination vary depending on the silica (SiO ₂ ) particle or the porosity. That is, according to the embodiment of the present invention, when the silica (SiO ₂ ) particle size and the porosity are in a suitable range, it is understood that not only the contamination but also the time required for vacuum digging is short. In addition, when the pressure regulating member is not provided as in Comparative Example 4, the degree of contamination is extremely high.

FIG. 5 is a schematic view of a vacuum deposition chamber using a pressure regulating member according to an embodiment of the present invention. In the vacuum deposition chamber, a DC / RF source 510 for DC / A substrate 520 which is an evaporation object disposed directly above the RF source, a pressure regulating member 530 disposed around the DC / RF source and communicating with the periphery of the DC / RF source and the outside of the chamber, a pressure regulating member 530 for generating plasma, And a pressure regulating member 550 disposed at a predetermined distance from the substrate and communicating with the inside and the outside of the chamber to evacuate the vacuum state inside the chamber.

Claims (16)

Silica (SiO ₂ ) particles having an average particle size of 1 to 50 μm; And
And tetraethyl orthosilicate (TEOS) for bonding the silica particles,
And a porosity of 25% to 40%.
The method according to claim 1,
Wherein the pressure regulating member has a density of 1.4 g / cm &lt; 3 &gt; to 1.6 g / cm &lt; 3 &gt;.
The method according to claim 1,
Wherein the pressure regulating member comprises 0.5 to 15 parts by weight of tetraethyl orthosilicate per 100 parts by weight of the silica particles.
delete delete delete A first step of obtaining a mixture comprising silica particles having an average particle size of 1 to 50 占 퐉, tetraethyl orthosilicate for bonding the silica particles, and polyvinyl alcohol for forming pores;
A second step of drying the mixture;
A third step of compression molding the dried mixture to obtain a molded body; And
And a fourth step of baking the molded body.
delete delete 8. The method of claim 7,
Wherein the second step comprises drying the mixture at 80 ° C to 100 ° C.
8. The method of claim 7,
Wherein the third step comprises compression molding the dried mixture at a pressure of 1.5 MPa to 20 MPa.
8. The method of claim 7,
Wherein the fourth step is a step of firing the formed body at a temperature of 1,000 ° C to 1,500 ° C.
A pressure regulating member according to any one of claims 1 to 3; And
And a connection pipe connected to an end of the pressure regulating member.
14. The method of claim 13,
Wherein the connecting tube is made of a quartz material.
A vacuum deposition chamber in which a gas inlet is formed; And
The vacuum vapor deposition apparatus according to any one of claims 1 to 3, further comprising a pressure regulating member provided at the gas inlet.
A vacuum deposition chamber in which a gas inlet is formed; And
The vacuum evaporation apparatus according to claim 13, further comprising a pressure regulating unit provided at the gas inlet.

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