WO2017195311A1 - Dispositif de cuisson et procédé de cuisson pour matériau de cible de pulvérisation cylindrique - Google Patents

Dispositif de cuisson et procédé de cuisson pour matériau de cible de pulvérisation cylindrique Download PDF

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Publication number
WO2017195311A1
WO2017195311A1 PCT/JP2016/064097 JP2016064097W WO2017195311A1 WO 2017195311 A1 WO2017195311 A1 WO 2017195311A1 JP 2016064097 W JP2016064097 W JP 2016064097W WO 2017195311 A1 WO2017195311 A1 WO 2017195311A1
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Prior art keywords
firing
furnace
sputtering target
cylindrical sputtering
target material
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PCT/JP2016/064097
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English (en)
Japanese (ja)
Inventor
久保田　善明
稔裕 森岡
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株式会社広築
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Application filed by 株式会社広築 filed Critical 株式会社広築
Priority to CN201680002852.1A priority Critical patent/CN107614739B/zh
Priority to KR1020177004552A priority patent/KR101892877B1/ko
Priority to JP2016555619A priority patent/JP6198363B1/ja
Priority to PCT/JP2016/064097 priority patent/WO2017195311A1/fr
Priority to TW106108715A priority patent/TWI636227B/zh
Publication of WO2017195311A1 publication Critical patent/WO2017195311A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B1/00—Shaft or like vertical or substantially vertical furnaces
    • F27B1/005—Shaft or like vertical or substantially vertical furnaces wherein no smelting of the charge occurs, e.g. calcining or sintering furnaces
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
    • C04B35/457—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates based on tin oxides or stannates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B1/00—Shaft or like vertical or substantially vertical furnaces
    • F27B1/10—Details, accessories, or equipment peculiar to furnaces of these types
    • F27B1/12—Shells or casings; Supports therefor
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B1/00—Shaft or like vertical or substantially vertical furnaces
    • F27B1/10—Details, accessories, or equipment peculiar to furnaces of these types
    • F27B1/20—Arrangements of devices for charging
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D3/00—Charging; Discharging; Manipulation of charge
    • F27D3/12—Travelling or movable supports or containers for the charge

Definitions

  • the present invention relates to a cylindrical sputtering target material firing apparatus, and more particularly, to produce a long cylindrical sputtering target used when a transparent conductive film used for a liquid crystal display element, a solar battery, or the like is manufactured by a sputtering method.
  • the present invention relates to a firing apparatus for an oxide fired body.
  • the transparent conductive film Since the transparent conductive film has high conductivity and high transmittance in the visible light region, it is used for liquid crystal display elements, solar cells, and other various light receiving element electrodes. As a transparent conductive film, a film having high transmittance and low resistance can be obtained. Therefore, a tin oxide-indium oxide film (ITO film), an aluminum oxide-zinc oxide film (AZO film), an indium oxide-gallium oxide-zinc oxide film. A system film (IGZO film) is widely used.
  • a sputtering method is used as a method for producing a transparent conductive film made of such an oxide film.
  • 100% argon gas of about 10 Pa or less is generally introduced, a sputtering target that is a raw material of the film is set on the cathode, and argon plasma is generated in a state where the substrate is set parallel to the target, Particles of the target component that are blown off when the argon cation collides with the target are deposited on the substrate to form a film.
  • magnetron sputtering is employed in which sputtering is performed while applying a magnetic field to the cathode.
  • a cylindrical sputtering target is adopted, a magnetic field generating facility and a cooling facility are installed inside the cylindrical backing tube, and sputtering is performed while rotating the cylindrical sputtering target.
  • the target The efficiency of use can be increased to 60-70%.
  • One method for producing this cylindrical sputtering target is a sintering method.
  • the sintering method water, a binder, and a dispersant are added to the raw material oxide powder and mixed to form a slurry, which is granulated with a spray dryer, etc., and then subjected to cylindrical sputtering with a cold isostatic press (CIP method).
  • CIP method cold isostatic press
  • the target is molded, and the resulting molded body is fired and molded at normal pressure in a high-temperature atmosphere in which an oxygen-containing gas flows, and a high-density target having a relative density of 90% or more can be produced.
  • the density is high, the bulk uniformity is high, and defects such as cracks, cracks and deformation are suppressed not only during firing but also in the manufacturing process and sputtering of a cylindrical sputtering target after firing.
  • Prior art for obtaining a quality oxide sintered body for a cylindrical sputtering target is disclosed.
  • JP 2012-125857 A ([0019-0021], [0024-0026], [FIG. 1])
  • the prior art is a rectangular electric furnace having a cylindrical sputtering target molded body having a size of 15 cm diameter ⁇ 20 cm length to 20 cm diameter ⁇ 30 cm length, and is directed upward from below in the furnace.
  • the atmospheric gas such as oxygen gas
  • the flow of oxygen-containing gas is uneven in the height direction in the furnace and inside and outside of the molded body, and the furnace temperature distribution is uneven.
  • the gas flow is made, the furnace temperature distribution is made uniform, and the sintering proceeds uniformly.
  • a highly uniform cylindrical oxide sintered body can be obtained.
  • the cylindrical sputtering target obtained by the prior art has a length of 20 to 30 cm.
  • 5 to 10 pieces are used.
  • bonding between the targets is performed by bonding.
  • the level difference of the divided portion which is the bonding is 0.5 mm or less. Therefore, when the number of divisions is increased, the number of occurrences of arcing is increased, cracking due to the divided portions is likely to occur, and there is a problem in that it takes time and labor for bonding, resulting in poor production efficiency.
  • a firing furnace having a low furnace height has been used for firing conventional flat sputtering target materials and short cylindrical sputtering target materials.
  • These firing furnaces are of a type in which a plate-like or short cylindrical sputtering target material, which is an object to be fired, is carried into the furnace and transferred into the furnace for firing.
  • this furnace is applied to firing a long cylindrical sputtering target material, when carrying a long object to be fired into the furnace, it is necessary to completely prevent falling and tilting. It was not achieved, and in the worst case, it could fall down and be damaged.
  • the present invention solves these problems, and when firing a plurality of long cylindrical sputtering target materials standing up and firing, without destroying the long fired object, It is an object of the present invention to provide a firing apparatus and a firing method that can be fired with less quality variation in the height and radial direction.
  • a firing apparatus for a cylindrical sputtering target material according to claim 1 of the present invention is a firing apparatus for a long cylindrical sputtering target material having a length of 1.5 to 2 m.
  • the firing furnace body provided and the firing furnace body placed on a traveling carriage, the firing that enables the rail travel to a position where the firing furnace body is separated from the position containing the fixed hearth and retracted
  • a furnace traveling device, and a furnace shell door that is openable and closable so as not to interfere when the fixed hearth is included is provided on one side surface of the firing furnace main body, and a lower part of the furnace shell and the fixed furnace Air leakage prevention between the floor edge Lumpur portion is provided, at the time of firing is characterized in that a furnace sealing lifting device for sealing by pressure contact seal portion by downward moving the sintering furnace main body.
  • the cylindrical sputtering target material according to the present invention is a long cylindrical sputtering target material having a diameter of 150 to 300 mm, a thickness of about 10 mm, and a length of 1.5 to 2 m. This calcination is performed at a high temperature of 1250 to 1700 ° C. for 3 to 30 hours in an oxygen atmosphere.
  • the firing furnace body travels to the firing position and surrounds the fixed hearth, but the furnace shell door of the firing furnace is fully opened so that it travels without damaging the cylindrical sputtering target material. And can be fired.
  • a furnace seal elevating device that prevents the gap between the firing furnace main body and the fixed hearth can be provided, and the seal between the inside of the furnace and the outside of the furnace can be performed completely. It is possible to appropriately maintain a high firing temperature. Thus, a long cylindrical sputtering target having a uniform and appropriate quality can be obtained by firing.
  • a cylindrical sputtering target material firing apparatus is the cylindrical sputtering target material firing apparatus according to claim 1, wherein the furnace seal lifting device supports a furnace at a lower portion of the firing furnace body.
  • the four support beams and the geared reduction device connected to the four support beams are provided, and each geared reduction device is driven from a single lifting / lowering geared motor through a driving force distribution device.
  • the geared reduction device is provided at four locations around the firing furnace, and the rotational force of one drive geared motor can be properly divided into four to apply the reduction of the seal portion. Sealing between the fixed hearths is performed appropriately and evenly, and the high-temperature furnace temperature can be appropriately maintained without being disturbed by air leakage.
  • cylindrical sputtering target material firing apparatus is the cylindrical sputtering target material firing apparatus according to claim 1 or 2, wherein a heater provided on the inner wall surface of the firing furnace includes an inner wall of each furnace. It is characterized by being arranged in three or more stages in the height direction.
  • cylindrical sputtering target material firing apparatus is the cylindrical sputtering target material firing apparatus according to claim 3, wherein the heater is a U-shaped ceramic heater made of MoSi 2.
  • a cylindrical sputtering target material firing apparatus is the cylindrical sputtering target material firing apparatus according to claim 3 or 4, wherein the heater is paired with an in-furnace thermometer. It is characterized by having installed.
  • the distribution of the firing temperature in the height direction in the firing furnace can be adjusted uniformly. Specifically, it is possible to control the temperature to a predetermined temperature by measuring the temperature of the area divided in the height direction with a thermometer installed therein and increasing or decreasing the heat output of the heater in the area. Normally, the tendency that the temperature in the furnace becomes higher at the higher temperature than at the lower temperature can be made to approach the predetermined temperature uniformly by adjusting the heat output for each zone. Thereby, there is no variation in the firing degree in the height (length) direction of the long cylindrical sputtering target material, which contributes to stable quality.
  • the MoSi 2 U-shaped ceramic heater is used as the heater, it has sufficient heat resistance and oxidation resistance at a maximum firing temperature of around 1700 ° C in an oxygen atmosphere, has a long life, and exhibits sufficient heating capacity. Therefore, it is optimal for firing a cylindrical sputtering target material that is fired for a long time.
  • the shape of the heater is U-shaped, it has a shape that can withstand the thermal expansion and contraction associated with the temperature rise and cooling of the heater, as well as each fractionated area divided in the height direction and the peripheral direction. This heater has an optimum shape in terms of heating strength and heating density.
  • the heater and the thermometer are arranged as a pair for each area, the temperature control for each of the divided areas in the height direction and the peripheral direction can be performed accurately and accurately.
  • the cylindrical sputtering target material firing apparatus is the cylindrical sputtering target material firing apparatus according to any one of claims 1 to 5, wherein the firing furnace main body has one or more upper portions.
  • a gas discharge hole is provided, and a plurality of oxygen blowing holes are provided in the height direction / periphery direction on the furnace inner wall from the lower part of the cylindrical sputtering target material on which the fixed hearth is placed.
  • the flow of oxygen in the firing furnace can be made uniform in the cross-sectional direction, and the difference in oxygen concentration at each location is minimized.
  • the furnace temperature distribution and the oxygen concentration distribution can be made uniform, so that the firing of the long cylindrical sputtering target material that is the object to be fired can proceed almost completely homogeneously, and the relative density can be stabilized.
  • the variation in relative density in the length direction and the cross-sectional direction can be substantially eliminated.
  • a method for firing a cylindrical sputtering target material according to claim 7 is a long object having a length of 1.5 to 2 m using the cylindrical sputtering target material firing device according to any one of claims 1 to 6.
  • One or a plurality of cylindrical sputtering target materials to be fired are placed on a fixed hearth in a state where they are self-supporting at predetermined intervals, and then the fixed hearth is taken into the center of the furnace. After the furnace shell door is opened and the firing furnace is moved from the retracted position to the firing position, the furnace shell door is closed, the temperature of the firing furnace is increased, and the temperature is raised to 1250 to 1700 ° C. in an oxygen atmosphere. And firing the object to be fired for 3 to 30 hours to obtain a cylindrical sputtering target.
  • the cylindrical sputtering target material firing method according to claim 8 is the cylindrical sputtering target material firing method according to claim 7, wherein the cylindrical sputtering target material is an ITO (tin oxide-indium oxide system) material, AZO ( It is characterized by being an aluminum oxide-zinc oxide system material or an IGZO (indium oxide-gallium oxide-zinc oxide system) material.
  • ITO titanium oxide-indium oxide system
  • AZO It is characterized by being an aluminum oxide-zinc oxide system material or an IGZO (indium oxide-gallium oxide-zinc oxide system) material.
  • the cylindrical sputtering target material according to the present invention is a long cylindrical sputtering target material having a diameter of 150 to 300 mm, a thickness of about 10 mm, and a length of 1.5 to 2 m.
  • This firing is performed with an ITO material at a high temperature of 1450 to 1700 ° C., preferably at a high temperature of 1500 to 1600 ° C., and with an AZO or IGZO material at a high temperature of 1250 to 1500 ° C., preferably at a temperature of
  • the reaction is performed at a high temperature of 1300 to 1450 ° C. in an oxygen atmosphere for 3 to 30 hours, preferably 5 to 10 hours. If this time is too long, the sintered structure may be enlarged and easily cracked.
  • the rate of temperature rise to the target firing temperature in firing is 100 to 500 ° C./Hr, and the rate of temperature drop from the target firing temperature is 10 to 150 ° C./Hr.
  • the cylindrical sputtering target material which is an object to be fired
  • the firing furnace moves from the standby position to the firing position to perform firing, so that the object to be fired is tilted by movement and the distance from the heating source does not change, and there is a risk of damage due to movement. No, the firing quality of the object to be fired can be obtained stably.
  • heating from the furnace wall from four directions is installed by dividing the heater in the height direction, making it easy to adjust the temperature distribution in the furnace height direction to be a long cylindrical sputtering target. Contributes to stable and improved firing quality.
  • the number and position of oxygen inflow and outflow for adjusting the oxygen atmosphere are arranged so that a uniform flow can be obtained with respect to the object to be fired.
  • the oxygen concentration and the firing temperature can be stably applied to the long cylindrical sputtering target material as intended.
  • the firing apparatus and firing method of the cylindrical sputtering target material of the present invention it is easy to make a long cylindrical sputtering target corresponding to the target quality, and the equipment is not excessive.
  • the baking apparatus is configured by compactly integrating facilities that have been used, has a small installation area, does not have a large facility cost, and is environmentally superior with no air pollution.
  • a 1.5 to 2 m long cylindrical sputtering target can be easily made with high quality, it can be used to manufacture a transparent conductive film for a large liquid crystal display device or a large photovoltaic power generation device. An optimum sputtering target with high use efficiency can be provided.
  • FIG. 1 is a schematic layout diagram of a firing apparatus for a cylindrical sputtering target material according to an embodiment for carrying out the present invention, and is a layout (cross section) diagram at the time of firing.
  • FIG. 2 is an arrangement (cross-sectional) view at the time of saving in FIG.
  • FIG. 3 is a schematic cross-sectional view taken along the line AA in FIG. 4 is a schematic cross-sectional view taken along the line BB in FIG.
  • firing apparatus 1 for a cylindrical sputtering target material according to the present invention will be described with reference to FIGS.
  • the cylindrical sputtering target material M used in the firing apparatus and firing method of the cylindrical sputtering target material according to the present invention is a long cylindrical sputtering material having a diameter of 150 to 300 mm, a wall thickness of around 10 mm, and a length of 1.5 to 2 m.
  • Target material is an ITO (tin oxide-indium oxide system) material, an AZO (aluminum oxide-zinc oxide system) material, or an IGZO (indium oxide-gallium oxide-zinc oxide system) material.
  • This baking is performed at a high temperature of 1450 to 1700 ° C.
  • the reaction is performed at a high temperature of 1300 to 1450 ° C. in an oxygen atmosphere for 3 to 30 hours, preferably 5 to 10 hours.
  • the temperature increase rate in the firing is 100 to 500 ° C./Hr, and the temperature decrease rate is 10 to 150 ° C./Hr.
  • FIG. 1 is a schematic plan view of the firing apparatus 1 and shows the layout during firing.
  • a firing furnace main body 2 that takes in a fixed hearth 3 on which four of the objects M to be fired, which are cylindrical sputtering target materials, are placed in a standing state is loaded on the firing furnace traveling device 4 and travels. It can run on rail 4-3.
  • the firing furnace body 2 has three sides of the furnace shell 2-c and the furnace wall refractory 2-a so as to surround the fixed hearth 3 from the surrounding four sides under the center portion, and the remaining one surface can be opened and closed.
  • the inside of the firing furnace body 2 is refractory.
  • a furnace ceiling refractory 2-b at the top of the furnace, and thus the inside of the firing furnace body 2 is refractory. Lined with objects.
  • a high-temperature and oxidation-resistant regular or irregular refractory material such as alumina or magnesia is used, and a conventional heat insulation is used on the furnace shell side.
  • the fixed hearth 3 is a quadrangular prism-shaped refractory, and a high-temperature and oxidation-resistant regular or irregular refractory material such as alumina and magnesia is used. .
  • the firing temperature at the lower end of the object to be fired M can be maintained by inserting the placing table 3-a between them, and the firing quality is maintained. easy.
  • the mounting table 3-a it is preferable to use a refractory having the same properties as the fixed hearth 3.
  • FIG. 2 shows that the firing furnace main body 2 of the firing apparatus 1 has moved from the fixed hearth 3 to a standby position.
  • the fixed hearth 3 is in an uncovered state, in which the object to be fired M is loaded or placed, or the fired object M to be fired is taken out, and there are no obstacles around the work. Therefore, the operation can be easily and reliably performed.
  • the firing furnace main body 2 has the open / close door 2-2 fully opened, and can be easily moved away from the fixed hearth 3 without hindrance. Further, when moving the firing furnace body 2, it is necessary to operate the furnace seal lifting device 5 to release the furnace seal.
  • the firing furnace traveling device 4 will be described with reference to FIGS. 3 and 4.
  • the firing furnace body 2 is mounted on the traveling carriage 4-4 via the four support beams 5-5.
  • the traveling carriage 4-4 includes a total of four traveling wheels 4-2 mounted on two traveling rails 4-3, and one of the traveling wheels 4-2 on each side is rotationally driven by a drive geared motor 4-1.
  • the traveling carriage 4-4 can automatically travel between a predetermined distance by a proximity switch corresponding to the firing position and the retreat position of the firing furnace body 2 provided on the traveling rail 4-3. .
  • the firing furnace body 2 travels to the firing position in FIG. 1,
  • the fixed hearth 3 is stopped in the state of being taken into the furnace and then the door 2-2 is closed, as shown in FIGS. 3 and 4, the lower part of the firing furnace body 2 and the outer periphery of the fixed hearth 3 are separated. A step-like gap is provided between them.
  • the furnace seal is completed by closing the firing furnace body 2 by closing the gap.
  • the furnace seal lifting / lowering device 5 includes one drive geared motor 5-1, drive shaft 2, two drive force distribution devices 5-3, and four geared reduction devices 5-4.
  • the output of one drive geared motor 5-1 is first distributed to an output shaft 5-2 perpendicular to the main shaft 5-2 by one drive force distribution device 5-3, and one output shaft 5-2 is Connected to two geared reduction devices 5-4.
  • Another orthogonal output shaft 5-2 is connected to the two geared reduction devices 5-4 via the orthogonal output shaft 5-2 by the driving force distribution device 5-3.
  • the four geared reduction devices 5-4 are connected to the support beams 5-5 to move the firing furnace body 2 up and down, and firing. Implementation and release of the furnace seal between the furnace body 2 and the fixed hearth 3 can be performed.
  • the open / close door 2-2 attached to the firing furnace body 2 is provided on the entire furnace side surface opposite to the retracting movement direction of the firing furnace body 2.
  • the open / close door 2-2 has a single-open structure that revolves around an open / close shaft 2-2a attached to the furnace shell so that it does not interfere with the fixed hearth 3 when the firing furnace body 2 moves. Can be fully opened.
  • the furnace wall of the open / close door 2-2 is provided with a door refractory 2-2c, and further protrudes from the door refractory 2-2c, and is heated in four stages in the height direction. A total of 2-e is provided. Opening and closing of the open / close door 2-2 can be performed manually or automatically. However, in the case of automatic, it is necessary to interlock the position information of the firing furnace body 2 and the fixed hearth 3.
  • the firing furnace body 2 will be described with reference to FIGS.
  • the firing furnace body 2 bakes a long cylindrical sputtering target material having a length of 150 to 300 mm ⁇ 1.5 to 2 m in an oxygen atmosphere at a set temperature in the range of 1250 to 1700 ° C. for 3 to 30 hours.
  • the in-furnace dimensions of the firing furnace body 2 are approximately 1.1 m square ⁇ 2.2 m height.
  • the present invention is not restricted by this number, and can uniformly apply radiation and convection heat transfer to the objects to be fired.
  • the present invention is applicable as long as it has an array of 2 ⁇ N columns.
  • the firing furnace body 2 has three sides of the furnace shell 2-c on the side surface, and the remaining one surface is constituted by an open / close door 2-2.
  • the furnace inner sides of the furnace shell 2-c and the open / close door 2-2 are lined with a furnace wall refractory 2-a and a door refractory 2-2c, respectively.
  • the inner wall of the ceiling portion of the firing furnace body 2 is made of the furnace ceiling refractory 2-b.
  • a high-temperature and oxidation-resistant regular or irregular refractory material such as alumina or magnesia is used, and a conventional heat insulation is used on the furnace shell side.
  • the heater 2-d is provided with a terminal portion in the furnace shell 2-c or the like and penetrates the furnace wall refractory 2-a and the door refractory 2-2c.
  • the heater part is provided in a form protruding from the furnace inner surface.
  • the heater 2-d is provided in four stages in the furnace height direction.
  • the heater 2-d is preferably a U-shaped ceramic heater made of MoSi 2 and has sufficient heat resistance and oxidation resistance at a maximum firing temperature of about 1700 ° C. in an oxygen atmosphere, has a long life, and exhibits sufficient heating capacity. Therefore, it is optimal for firing the cylindrical sputtering target material M that is fired for a long time.
  • the heater 2-d since the shape of the heater 2-d is U-shaped, the heater 2-d has a shape that can withstand thermal expansion and contraction caused by temperature rise and cooling of the heater 2-d, and is divided in the height direction and the peripheral direction. As the heater 2-d for each fractionated area, it has an optimum shape in terms of heating strength and heating density
  • a furnace thermometer 2-e is inserted from the furnace shell 2-c into the furnace at the center of each stage of the heater 2-d and disposed in pairs with the heater 2-d.
  • the internal temperature can be measured.
  • distribution of the baking temperature of the height direction in the furnace of the baking furnace main body 2 can be adjusted uniformly.
  • the temperature of the zone divided in the height direction is measured by the furnace thermometer 2-e installed there, and the heat output of the heater 2-d in that zone is increased or decreased.
  • thermometer 2-e a well-known platinum rhodium thermocouple can be used.
  • one or a plurality of gas discharge holes 2- are formed in the upper part of the firing furnace body 2 so that the inside of the firing furnace body 2 is maintained in an oxygen atmosphere and the firing temperature is kept at a specified level.
  • g and a plurality of oxygen blowing holes in the height direction / peripheral direction from the lower part of the cylindrical sputtering target material M on the fixed hearth and from the furnace inner walls 2-b and 2-2c (Not shown).
  • the furnace temperature distribution and the oxygen concentration distribution can be made uniform, so that the firing of the long cylindrical sputtering target material M, which is an object to be fired, can proceed almost completely homogeneously, and the relative density can be increased. While improving stably, the variation of the relative density of a length direction or a cross-sectional direction can be substantially eliminated.
  • the cylindrical sputtering target material a material selected from an ITO (tin oxide-indium oxide system) material, an AZO (aluminum oxide-zinc oxide system) material, or an IGZO (indium oxide-gallium oxide-zinc oxide system) material can be used.
  • the cylindrical sputtering target material is prepared by adding water, a binder and a dispersant to the raw material oxide powder, mixing it into a slurry, granulating it with a spray dryer, etc., and then cold isostatic pressing (CIP method), etc. Can be molded and manufactured.
  • the cylindrical sputtering target material is a long cylindrical sputtering target material having a diameter of 150 to 300 mm, a thickness of around 10 mm, and a length of 1.5 to 2 m.
  • the firing method of the cylindrical sputtering target material is performed as follows.
  • a fixed furnace in which a single or a plurality of (four in the figure) objects to be fired of a cylindrical sputtering target material M having a length in the range of 1.5 to 2 m are self-supported at predetermined intervals.
  • the open / close door 2-2 of the firing furnace body 2 was opened so that the fixed furnace floor 3 was taken into the center of the furnace, and the firing furnace body 2 was moved from the retracted position to the firing position. Thereafter, the open / close door 2-2 is closed, the firing furnace body 2 is heated, and the object M is fired at a high temperature of 1250 to 1700 ° C. in an oxygen atmosphere for 3 to 30 hours.
  • a shaped sputtering target can be obtained.
  • This firing is performed with an ITO material at a high temperature of 1450 to 1700 ° C., preferably at a high temperature of 1500 to 1600 ° C., and with an AZO or IGZO material at a high temperature of 1250 to 1500 ° C., preferably at a temperature of
  • the reaction is performed at a high temperature of 1300 to 1450 ° C. in an oxygen atmosphere for 3 to 30 hours, preferably 5 to 10 hours. If this time is too long, the sintered structure may be enlarged and easily cracked.
  • the rate of temperature rise to the target firing temperature in the firing process is 100 to 500 ° C./Hr, and the rate of temperature drop after firing is 10 to 150 ° C./Hr.
  • the sintered cylindrical sputtering target is bonded to a backing tube with a built-in magnetic field generation facility and cooling facility by bonding, magnetron sputtering is performed, and the target oxide is deposited on the substrate by this sputtering. And a transparent conductive film used for solar cells and the like can be reliably and stably manufactured.
  • Cylindrical sputtering target material firing device 2 Firing furnace body 2-a: Furnace wall refractory 2-b: Furnace ceiling refractory 2-c: Furnace shell 2-d: Heater 2-e: In-furnace thermometer 2-f: Oxygen inlet 2-g: Oxygen outlet 2-2: Open / close door 2-2a: Opening and closing shaft 2-2b: Closing handle 2-2c: Door refractory 3: Fixed hearth 3-a: Mounting table 4: Firing furnace traveling device 4-1: Drive geared motor 4-2: Traveling wheel 4-3: Traveling rail 4-4: Traveling cart 5: Furnace seal lifting device 5-1 Drive geared motor 5-2: Drive shaft 5-3: Drive power distribution device 5-4: Geared pressure reduction Equipment 5-5: Support beam M: Object to be fired (cylindrical sputtering target material)

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Metallurgy (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Resistance Heating (AREA)
  • Furnace Charging Or Discharging (AREA)
  • Furnace Details (AREA)

Abstract

Le problème décrit par la présente invention porte sur un dispositif de cuisson pour fabriquer une cible de pulvérisation cylindrique allongée qui est utilisée pour la fabrication, par pulvérisation, d'un film conducteur transparent utilisé dans un dispositif d'affichage à cristaux liquides, une cellule solaire et analogue. La solution selon la présente invention est caractérisée en ce qu'elle comporte : un foyer fixe dans lequel un élément à cuire du matériau de cible de pulvérisation cylindrique allongée est placé verticalement; un corps de four de cuisson centré autour du foyer fixe et présentant, sur les parois du four, une pluralité de chauffages et un orifice d'entrée d'oxygène; et un mécanisme grâce auquel le corps du four de cuisson est placé sur un chariot mobile et peut se déplacer par rail entre une position de cuisson et une position d'attente, le mécanisme ouvrant et fermant en outre une fermeture étanche de four entre le fond du four de cuisson et le foyer fixe.
PCT/JP2016/064097 2016-05-12 2016-05-12 Dispositif de cuisson et procédé de cuisson pour matériau de cible de pulvérisation cylindrique WO2017195311A1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
CN201680002852.1A CN107614739B (zh) 2016-05-12 2016-05-12 圆柱形溅射靶材的焙烧装置以及焙烧方法
KR1020177004552A KR101892877B1 (ko) 2016-05-12 2016-05-12 원통형 스퍼터링 타겟재의 소성 장치 및 소성 방법
JP2016555619A JP6198363B1 (ja) 2016-05-12 2016-05-12 円筒形スパッタリングターゲット材の焼成装置及び焼成方法
PCT/JP2016/064097 WO2017195311A1 (fr) 2016-05-12 2016-05-12 Dispositif de cuisson et procédé de cuisson pour matériau de cible de pulvérisation cylindrique
TW106108715A TWI636227B (zh) 2016-05-12 2017-03-16 圓筒形濺鍍靶材之煅燒裝置及煅燒方法

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CN108097530A (zh) * 2018-01-19 2018-06-01 广西晶联光电材料有限责任公司 一种平面靶材背面金属化设备及方法
CN111485218A (zh) * 2020-04-22 2020-08-04 广东生波尔光电技术有限公司 特种工件辅助镀膜的自动控制系统
CN114107929A (zh) * 2021-11-29 2022-03-01 青岛科技大学 一种可预热溅射靶材的旋靶管装置

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CN109706285B (zh) * 2018-11-29 2020-07-31 沧州中铁装备制造材料有限公司 冶炼炉转接炉用的底部防飞溅的收集座装置

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CN114107929A (zh) * 2021-11-29 2022-03-01 青岛科技大学 一种可预热溅射靶材的旋靶管装置

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CN107614739A (zh) 2018-01-19
TWI636227B (zh) 2018-09-21
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