WO2013001827A1 - 加熱装置、真空加熱方法及び薄膜製造方法 - Google Patents
加熱装置、真空加熱方法及び薄膜製造方法 Download PDFInfo
- Publication number
- WO2013001827A1 WO2013001827A1 PCT/JP2012/004212 JP2012004212W WO2013001827A1 WO 2013001827 A1 WO2013001827 A1 WO 2013001827A1 JP 2012004212 W JP2012004212 W JP 2012004212W WO 2013001827 A1 WO2013001827 A1 WO 2013001827A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- heating
- gap
- heater
- storage container
- container
- Prior art date
Links
Images
Classifications
-
- 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
- C23C14/24—Vacuum evaporation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
-
- 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
- C23C14/24—Vacuum evaporation
- C23C14/243—Crucibles for source material
-
- 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
- C23C14/24—Vacuum evaporation
- C23C14/26—Vacuum evaporation by resistance or inductive heating of the source
-
- 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
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
- C23C14/562—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks for coating elongated substrates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/04—Construction or manufacture in general
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Definitions
- the present invention relates to a heating device, a vacuum heating method, and a thin film manufacturing method.
- Nonaqueous electrolyte secondary batteries are attracting attention as secondary batteries that can satisfy this requirement.
- silicon (Si), germanium (Ge), tin (Sn) or the like may be used as an electrode active material (hereinafter simply referred to as “active material”) Proposed.
- Si or Sn is a simple substance of silicon, a silicon alloy, a compound containing silicon and oxygen, a compound containing silicon and nitrogen, a simple substance of tin, a tin alloy, a compound containing tin and oxygen, and a compound containing tin and nitrogen
- active material when used as an active material, they are accompanied by expansion due to a large change in crystal structure when storing lithium ions.
- the active material particles are broken or the active material layer is peeled off from the current collector, the electron conductivity between the active material and the current collector is lowered, and as a result, the cycle characteristics are lowered. there were.
- the active material containing these Si or Sn has a problem of irreversible capacity. That is, when an active material containing Si or Sn is used for the negative electrode, a part of lithium ions occluded at the time of initial charge is not released from the negative electrode at the time of discharge, resulting in a problem of reduced battery capacity.
- Patent Document 1 discloses a method of applying lithium to an active material layer formed on the surface of a current collector by vacuum evaporation.
- vacuum deposition technology is applied to the manufacture of organic EL displays.
- Patent Document 2 an evaporation material storage unit and a nozzle connected to the storage unit and ejecting the evaporation material as an evaporation source for depositing a low molecular weight organic material capable of evaporation at a relatively low temperature of 200 to 400 ° C.
- An evaporation source is described which comprises a part and a heating part surrounding the storage part.
- Patent Document 3 describes an evaporation source in which an indirectly heated heater is disposed in contact with the bottom of a crucible as an evaporation source of a metal such as aluminum, copper, silver, or zinc. This evaporation source is used when the temperature at evaporation is as high as 1000 ° C. or more.
- Patent Document 4 a box-shaped inner patch holding high temperature molten metal, a crucible body, and a spacer interposed between the inner patch and the crucible main body are provided, and between the inner patch and the crucible main body A crucible filled with a liquid heat carrier in the space of This crucible is used when heating and melting the vapor deposition material directly by a technique such as an electron gun.
- a heating device that can be used in a vacuum is required. It is not easy to heat an object efficiently in a vacuum because the gas serving as a medium is lean in vacuum. For example, if a heater (heating body) is integrated with a crucible (heating body), it may be possible to improve the heat transfer efficiency from the heating body to the heating body by direct contact. However, if the heat transfer efficiency is emphasized too much, the maintainability is likely to deteriorate.
- the present invention aims to provide a heating device capable of efficiently heating an object in a vacuum and easy maintenance.
- a heating body configured to be separable from the body to be heated and having a gap formed between itself and the body to be heated, and a gas introduction path for introducing a heat transfer gas into the space; Equipped with The to-be-heated body provides a heating apparatus heated by the heating body via the heat transfer gas.
- the heating body can be separated from the body to be heated. Therefore, both can be easily maintained.
- a gap is formed between the body to be heated and the heating body.
- the heat transfer gas is introduced into the gap through the gas introduction path.
- the body to be heated is heated by the heating body via the heat transfer gas. Therefore, the object to be heated such as the crucible can be efficiently heated.
- Sectional drawing which shows typically the vapor deposition apparatus of 1st embodiment of this invention
- the partial enlarged view which expands and shows the vapor deposition source vicinity of the vapor deposition apparatus of FIG. 1
- the partial enlarged view which expands and shows the vapor deposition source vicinity applicable to the vapor deposition apparatus of FIG. 1
- FIG. 23 is a perspective view of a bowl-like part that can be used for the evaporation source shown in FIG. Cross section of evaporation source according to modification 3
- the first aspect of the present disclosure is An object to be heated in vacuum, A heating body configured to be separable from the body to be heated and having a gap formed between itself and the body to be heated, and a gas introduction path for introducing a heat transfer gas into the space; Equipped with The to-be-heated body provides a heating apparatus heated by the heating body via the heat transfer gas.
- the heating device of the first aspect may be configured as a vapor deposition device.
- the inventors have found the following problems in the conventional vapor deposition apparatus. By applying the heating apparatus of the first aspect to a vapor deposition apparatus, the following problems can be overcome.
- a nozzle type evaporation source as disclosed in Patent Document 2 is used.
- the deposition material needs to be heated to 600 ° C. or higher.
- the heating temperature of the heater has to be 1000 ° C. or more.
- the maximum operating temperature of the cartridge heater is 870 ° C
- the maximum operating temperature of the ceramic heater is 1100 ° C. Therefore, if heating is performed at 1000 ° C or higher using these heaters, the temperature control of the heater can be performed. The use of the heater has become extremely difficult.
- the inventors examined the deposition by heating several hundred grams of the deposition material stored in the crucible by directly attaching a cartridge heater as a heater to the outer surface of the crucible. At this time, the evaporation temperature under vacuum was predicted from the vapor pressure diagram of the vapor deposition material, and the heating temperature of the vessel was set. As a result, although a vapor deposition film could be formed on the substrate, it was necessary to remove the cartridge heater from the crucible in advance when performing maintenance such as removing the vapor deposition material remaining in the crucible after completion of vapor deposition. In particular, when the width of the substrate is wide and the deposition material to be stored increases, the capacity of the crucible also increases accordingly, the number of cartridge heaters increases, and the maintenance becomes extremely complicated.
- the inventors examined deposition by storing the crucible in a heating container having a heater, instead of directly attaching the heater to the crucible. According to this method, maintenance work after the end of deposition is facilitated, but the thermal conductivity of the heating vessel and the crucible is reduced under vacuum, so the temperature of the deposition material is sufficient in the above-mentioned heater operating temperature range There is a problem that the deposition can not be performed without raising the temperature, or even if the deposition can be performed, the deposition can not be controlled if the deposition is continuously performed for a long time.
- the object to be heated is a storage container that holds a deposition material and has an opening through which the evaporated deposition material passes.
- the heating body detachably houses the storage container, and includes a heater for heating the deposition material in the storage container, through which the deposition material evaporated from the storage container passes. And the outer wall surface of the storage container and the inner wall surface of the heating container directly face each other when the storage container is stored, so that the gap is generated between the inner wall surface and the outer wall surface.
- a heating vessel configured as The heating device further comprises: (i) a vacuum chamber for accommodating the storage container and the heating container, and for internally depositing on the substrate, and (ii) a vacuum pump for evacuating the vacuum chamber.
- the heating apparatus is provided.
- the second aspect is A storage container for holding a deposition material and having an opening through which the evaporated deposition material passes;
- a heating container for removably storing the storage container and having a heater for heating the deposition material in the storage container, the heating container having an opening through which the deposition material evaporated from the storage container passes
- the gap is generated between the inner wall surface and the outer wall surface by the outer wall surface of the storage container and the inner wall surface of the heating container directly facing each other.
- a heating vessel A vacuum chamber for containing the storage container and the heating container and for depositing on the substrate inside;
- a vacuum pump for evacuating the vacuum chamber; To provide a vapor deposition apparatus.
- the storage container holding the vapor deposition material is stored in the heating container, and a gap is formed between the two containers.
- the storage container and the heating container can be easily separated when performing maintenance such as removing the deposition material remaining inside. Therefore, it is not necessary to perform troublesome work such as removing the heater from the storage container, and the maintenance work can be easily performed.
- the heat transfer gas is introduced into the gap, the heat from the heating vessel is efficiently transferred to the storage vessel during the vacuum deposition, and the deposition material is heated. Therefore, since the temperature of the vapor deposition material can be sufficiently raised while being indirect heating, it is possible to control vapor deposition continuously and stably for a long time.
- deposition can be carried out efficiently and continuously under vacuum, and maintenance work after completion of deposition can be dramatically simplified, so it is extremely excellent. Deposition can be performed with high productivity.
- the third aspect of the present disclosure provides the heating device according to claim 2, wherein in addition to the second aspect, the gap has a width of 0.5 mm or less. According to the third aspect, the gas pressure in the gap can be increased with a small gas introduction amount.
- the heating device further includes a suppression structure that suppresses the heat transfer gas from flowing out of the gap into the vacuum chamber.
- the pressure of the gap can be increased with a small amount of gas introduced.
- the reduction of the degree of vacuum in the vacuum chamber due to the introduction of the gas into the gap can be avoided.
- the suppression structure is configured to change the traveling direction of the heat transfer gas flowing out of the gap, or the heat transfer flowing out of the gap
- a heating device configured to reduce the amount of gas.
- the pressure in the gap can be increased with a small amount of gas introduced.
- the reduction of the degree of vacuum in the vacuum chamber due to the introduction of the gas into the gap can be avoided.
- the suppression structure is a step structure provided around the opening of the storage container and the opening of the heating container, or Provided is a heating device which is a tapered structure.
- a heating device which is a tapered structure.
- alignment when storing the storage container in the heating container can be accurately performed, and a predetermined gap can be reliably ensured on the side surface and the bottom surface of the storage container.
- the gap may be closed at the opening of the storage container and the heating container and may be a space isolated from the vacuum chamber. In this case, the pressure in the gap can be increased with a small amount of gas introduced.
- the gap between the opening of the storage container and the opening of the heating container is A heating device is provided, which is formed to be narrower than the gap other than the periphery of the opening. According to the seventh aspect, diffusion of the gas introduced into the gap into the vacuum tank can be suppressed, and the pressure of the gap can be increased with a small amount of gas introduced.
- An eighth aspect of the present disclosure provides the heating device according to any one of the second to seventh aspects, wherein the thermal expansion coefficient of the heating container is smaller than the thermal expansion coefficient of the storage container. According to the eighth aspect, as the heater of the heating container heats up, the gap between the heating container and the storage container becomes smaller and the gas pressure in the gap is increased, so that the heat transfer coefficient becomes larger, and the heat efficiency is improved. It can be enhanced.
- the heat transfer gas is interposed between a space inside the heating vessel having the heater and an inner wall surface of the heating vessel.
- a heating device is provided, further comprising a passage for passing. According to the ninth aspect, the heat of the heater is more efficiently transferred to the storage container, so the amount of heating of the heater can be reduced.
- a tenth aspect of the present disclosure is the heating device according to any one of the second to ninth aspects, wherein the gap is closed at the opening of the storage container and the opening of the heating container. I will provide a.
- the pressure in the gap can be increased with a small amount of gas introduced. It can also be avoided that the degree of vacuum in the vacuum chamber is reduced (the pressure is increased) due to the gas introduction into the gap.
- An eleventh aspect of the present disclosure provides the heating device according to any one of the second to tenth aspects, wherein a lid is placed on the opening of the gap. According to the eleventh aspect, the presence of the lid suppresses the gas diffusion into the vacuum chamber, and the pressure of the gap can be increased with a small amount of gas introduced.
- a heating device in which a gas flow path for passing the heat transfer gas introduced into the gap is formed on the lower surface of the lid.
- the release point of the gas introduced into the gap into the vacuum chamber can be located away from the opening of the storage container. Therefore, the gas introduced into the gap leaks in the direction of the opening of the storage container, collides with the vapor deposition material evaporating from the storage container, and deteriorates the film quality (for example, the adhesion with the substrate becomes weak, or The effect on deposition such as causing a porous film) can be avoided.
- the thirteenth aspect of the present disclosure is A storage container for holding a deposition material and having an opening through which the evaporated deposition material passes;
- the heating container has a heater for releasably storing the storage container and heating the deposition material in the storage container, and having an opening through which the deposition material evaporated from the storage container passes.
- the outer wall surface of the storage container and the inner wall surface of the heating container directly oppose each other, so that a gap is generated between the inner wall surface and the outer wall surface.
- the thin film manufacturing method includes a step of evaporating the vapor deposition material from the storage container by heating the vapor deposition material in the storage container by the heater while introducing a heat transfer gas into the gap.
- deposition can be carried out efficiently and continuously under vacuum, and maintenance work after the end of deposition can be dramatically simplified, so extremely excellent productivity Deposition can be performed.
- the thin film manufacturing method provides the heat transfer gas introduction amount controlled in accordance with the pressure in the vacuum chamber. By appropriately controlling the amount of heat transfer gas introduced, it is possible to suppress the fluctuation of the evaporation rate of the deposition material.
- a fifteenth aspect of the present disclosure provides the thin film manufacturing method, in addition to the thirteenth or fourteenth aspect, wherein the deposition material is lithium and the heat transfer gas is an inert gas. According to the fifteenth aspect, lithium can be prevented from reacting with the heat transfer gas, and a high quality lithium thin film can be formed on the substrate.
- the inventors also disclose the following.
- a heating device for vacuum it is conceivable to use a heating device provided with a rod-shaped heater and a heating block having a slot for inserting the heater. Since it is difficult to obtain sufficient heat conduction in a vacuum, it is effective to bring the heater into close contact with the slot.
- the outer diameter of the heater substantially matches the inner diameter of the slot, it becomes impossible to pull the heater out of the heating block at the time of maintenance of the heater or replacement of the heater.
- the gap between the heater and the slot is too wide, the heat conduction from the heater to the heating block becomes insufficient, and the temperature rising characteristics of the heating block deteriorate. In this case, since it is necessary to raise the temperature of the heater, not only energy efficiency (power efficiency) is lowered, but also the life of the heater is shortened.
- the object to be heated is a heating block for heating an object in a vacuum
- the heating body is a rod-like heater detachably inserted into a slot formed in the heating block,
- the gap is formed between the slot and the heater,
- the gas introduction path provides a heating device formed in the heating block to introduce a heat transfer gas into the gap.
- the sixteenth aspect is A heating block for heating the object in a vacuum; A slot formed in the heating block; A rod-like heater removably inserted into the slot; A gas introduction path formed in the heating block for introducing a heat transfer gas into a gap between the slot and the heater; To provide a heating device.
- a gas introduction path is formed in the heating block.
- the heat transfer gas is introduced into the gap between the heater and the slot through the gas introduction path.
- the heat transfer from the heater to the heating block is promoted, so the difference between the temperature of the heater and the temperature of the heating block can be reduced. That is, the temperature rising characteristics of the heating block can be improved while appropriately securing the gap between the heater and the slot. Since the gap between the heater and the slot can be secured appropriately, the heater can be easily pulled out of the slot at the time of maintenance or replacement.
- a plurality of the slots are formed in the heating block, the heater is inserted into each of the plurality of slots, and the gas introduction path is A heating device is provided, including a first path for introducing the heat transfer gas into the slots from the outside of the heating block, and a second path for communicating the slots with each other. According to such a configuration, heat transfer from the heater to the heating block can be promoted with a small amount of heat transfer gas.
- the gap is relatively wide at a central portion in the longitudinal direction of the slot, and the gap is relatively large at an end in the longitudinal direction of the slot.
- the gap is relatively narrow at the end of the slot, leakage of the heat transfer gas from the gap can be reduced.
- the heater can be easily pulled out of the slot and can be easily inserted into the slot.
- a nineteenth aspect of the present disclosure is the method according to any one of the sixteenth to eighteenth aspects, wherein the heater includes a heater main body having a heating element, and the heat generation of the heater main body so as to supply power to the heating element.
- a heating device having a lead electrically connected to the body, the slot being closed on the side opposite to the side on which the lead is located. By sealing the slot, it is possible to reduce the amount of heat transfer gas leaking from the gap into the interior of the vacuum chamber.
- the flange provides the same effect as when the slot is formed by a bottomed hole.
- a twentieth aspect of the present disclosure is the method according to any one of the sixteenth to nineteenth aspects, wherein the dimensions of the heater and the dimensions of the slot are adjusted to allow movement of the heater when energized.
- a heating device Provided is a heating device. According to such a configuration, it is possible to prevent a large force (load or stress) from being applied to the heater due to thermal expansion at the time of energization. Therefore, the life of the heater is extended.
- a twenty-first aspect of the present disclosure is the lead portion according to any one of the sixteenth to twentieth aspects, wherein the heater includes a heater main body having a heating element, and a lead for supplying power to the heating element. And a connecting portion provided between the lead portion and the heater body so as to electrically connect the lead wire to the heating element, the connecting portion being located outside the slot. To provide a heating device. This can extend the life of the heater.
- a twenty-second aspect of the present disclosure is any one of the sixteenth to twenty-first aspects, wherein the heating device is an evaporation source, and the heating block has a recess for containing the object as a material to be evaporated.
- a heating device is provided, which is an evaporation vessel. The material contained in the recess can be melted and evaporated by heating the heating block with the heater.
- a twenty-third aspect of the present disclosure provides the heating device according to any one of the sixteenth to twenty-first aspects, wherein the heating device is a substrate heating device that heats a substrate. According to the twenty-third aspect, the substrate can be efficiently heated.
- the object can be efficiently heated in a vacuum.
- a twenty-fifth aspect of the present disclosure uses the heating apparatus according to any one of the sixteenth to twenty-second aspects to evaporate the material of the thin film as the object in a vacuum and to deposit the evaporated material on a substrate. Providing the heat transfer gas from outside the vacuum to the heating device while performing the deposition step. According to the twenty-fifth aspect, a high quality thin film can be efficiently produced.
- deposition is performed in a deposition area on a cooling can while conveying a sheet-like substrate in a chamber.
- FIG. 1 is a cross-sectional view schematically showing the vapor deposition apparatus of the first embodiment
- FIG. 2 is a partially enlarged view showing the vicinity of a vapor deposition source of the vapor deposition apparatus of FIG.
- the vapor deposition apparatus 100 is provided outside the chamber 2 (vacuum chamber) 2 and the exhaust pump 1 for evacuating the chamber 2 and a gas such as an inert gas from the outside of the chamber 2 to the inside of the chamber 2
- a gas introduction pipe 11 gas introduction path for introducing a heat transfer gas
- a mass flow controller 12 for adjusting a gas flow rate by the gas introduction pipe 11 are provided.
- the chamber 2 has a storage container 9 (heated body) for holding a vapor deposition material, and a heating container 10 (heater) for detachably storing the storage container 9 and heating the storage container 9.
- a shielding portion 13 for the purpose.
- the storage container 9 has a recess for holding the deposition material and an opening for passing the deposition material gas heated and vaporized by the heating container 10 on the upper end surface.
- a material which comprises the storage container 9 the material which does not react with the vapor deposition material at the time of heating evaporation is selected. In the present embodiment, the storage container 9 is not provided with the heating means.
- the storage container 9 is disposed such that the long side of the evaporation surface 9S is parallel to the width direction of the substrate 4.
- the storage container 9 may be configured such that the long side of the evaporation surface 9S has a sufficient length (for example, 600 mm or more when the width of the substrate 4 is 500 mm) with respect to the width of the substrate 4.
- the opening of the storage container 9 and the cooling can 6 are arranged as close as possible to the extent that the substrate 4 being transported does not come in contact with these members. Specifically, for example, a gap of about 3 mm can be provided. Thus, it is possible to prevent deposition contamination on members other than the substrate 4 in the chamber 2.
- the heating container 10 is a container that encloses the surface other than the opening of the storage container 9 and stores the storage container 9.
- the heating container 10 has an opening in the same direction as the opening of the storage container 9 when the storage container 9 is stored.
- the vapor deposition material gas to be evaporated passes through the opening of the heating vessel 10 and adheres to the substrate surface. Furthermore, attachment of the storage container 9 to the heating container 10 and removal of the storage container 9 from the heating container 10 are performed through the opening of the heating container 10. Therefore, the opening of the heating vessel 10 has a size that allows the storage vessel 9 to pass through.
- the heating container 10 may be designed to be divisible and the storage container 9 may be removed by dividing the heating container 10. In this case, the opening of the heating container 10 It does not have to pass the container 9.
- the upper end surface of the heating container 10 in the vertical direction and the upper end surface of the storage container 9 in the vertical direction are flush with each other so that the heat from the heating container 10 is transmitted to the storage container 9 without excess or deficiency.
- it is not necessarily limited to this.
- the heating container 10 As a material which comprises the heating container 10, it is desirable to select from the same material as the component of the storage container 9, and the material whose thermal expansion coefficient is smaller than the component of the storage container 9. In particular, it is desirable to use a material having a thermal expansion coefficient smaller than that of the storage container 9 as a component of the heating container 10. As a result, as the temperature of the heater built in the heating container 10 rises, the gap between the heating container 10 and the storage container 9 becomes smaller, and the gas pressure in the gap increases, so that the heat conduction coefficient becomes larger. Can be enhanced.
- a combination of components having different thermal expansion coefficients for example, a combination of SUS304 (1.73 ⁇ 10 ⁇ 5 / ° C.) and Inconel (1.15 ⁇ 10 ⁇ 5 / ° C.); SUS 304 or SUS 430 (1.04) ⁇ a 10 -5 / ° C.), carbon (0.5 ⁇ 10 -5 / °C) , or refractory metal, for example, Mo (0.49 ⁇ 10 -5 / °C ), tungsten (0.51 ⁇ 10 - 5 / ° C.), tantalum (0.65 ⁇ 10 ⁇ 5 / ° C.), combinations with niobium (0.7 ⁇ 10 ⁇ 5 / ° C.), and the like.
- thermal expansion coefficients are all mean thermal expansion coefficients of 0 to 100 ° C. Strictly speaking, attention should be paid to the average thermal expansion coefficient between room temperature and the maximum temperature reached of the heating vessel 10. However, except in special cases, the magnitude relation of the average thermal expansion coefficient between two solids at 0 to 100 ° C. is the magnitude of the average thermal expansion coefficient between two solids at room temperature to the highest achieved temperature of the heating vessel 10 Match the relationship.
- a heater 20 for heating the vapor deposition material is embedded in the components of the heating container 10.
- the heater 20 can heat the vapor deposition material held inside the storage container 9.
- a cartridge heater maximum operating temperature 870 ° C.
- a ceramic heater maximum operating temperature 1100 ° C.
- the heating container 10 is sized so as to create a gap 50 between the outer wall surface of the storage container 9 and the inner wall surface of the heating container 10 when the storage container 9 is stored.
- a gap 50 is formed by the outer peripheral surface of the storage container 9 and the inner wall surface of the heating container 10 facing each other directly.
- the gap 50 is a single layer gap.
- the outer wall surface of the storage container 9 and the inner wall surface of the heating container 10 are in contact, but in this case, when removing the storage container 9 from the heating container 10 Friction makes removal difficult. Furthermore, there is a concern that the seizing may make it difficult to separate the two containers.
- since the gap 50 exists between both containers there is no concern of burn-in, removal is easy, and maintenance work after the end of deposition can be easily performed.
- the gas pressure in the gap 50 is raised by introducing a gas into the gap 50 from the gas introduction pipe 11.
- the presence of the gas in the gap 50 facilitates the conduction of heat, and the heat from the heating vessel 10 can be transferred to the storage vessel 9 to carry out the deposition.
- the heat transfer coefficient from the heating vessel 10 to the storage vessel 9 is 0.002 W / cm 2 / K in a vacuum of 0.1 Pa or less.
- the heat transfer coefficient rises when the gas pressure in the gap 50 is 50 Pa or more, and for example, the heat transfer coefficient at 100 Pa in the gas pressure of the gap 50 is 0.01 W / cm 2 / K.
- the size of the gap 50 is desirably 1.0 mm or less. That is, it is desirable that the inner dimension of the recess of the heating container 10 be larger than the outer dimension of the storage container 9 in the range of 1.0 mm or less.
- the heat transfer coefficient under the same pressure has a gap dependency. For example, when the gap gas pressure is 100 Pa and the gap width is 0.5 mm, the heat transfer coefficient is 0.007 W / cm 2 / K, but if the gap becomes larger than this, the gas flow in the gap is increased even if the gas flow rate is increased. Since the pressure does not rise, it is difficult to obtain the effect of introducing the gas.
- the width of the gap 50 is more preferably 0.5 mm or less.
- the lower limit of the width of the gap 50 is not particularly limited as long as the storage container 9 can be easily removed from the heating container 10 and the storage container 9 can be easily attached to the heating container 10.
- the lower limit of the width of the gap 50 is, for example, 0.1 mm.
- the vapor deposition material contained in the storage container 9 is heated by the heater 20 through the heating container 10, and the gas is stored from the gas introduction pipe 11 using the mass flow controller 12. 9 is introduced into the gap 50 between the heating container 10 and the heating container 10. The heat from the heating vessel 10 is efficiently transferred to the storage vessel 9 by the gas present in the gap 50, and the vapor deposition material in the storage vessel 9 is heated and melted to evaporate from the evaporation surface 9S and be supplied to the surface of the substrate 4 Be done.
- the amount of gas introduced by the mass flow controller 12 is controlled so that the pressure of the vacuum gauge 40 attached to the chamber 2 becomes constant. It is desirable to control the gas introduction amount in accordance with the pressure in the chamber 2. By controlling the gas introduction amount so that the pressure in the chamber 2 becomes constant, it is possible to suppress the fluctuation of the evaporation rate due to the change of the degree of vacuum. Furthermore, since the gas pressure in the gap 50 between the heating container 10 and the storage container 9 can be made constant, heat conduction from the heating container 10 to the storage container 9 is stabilized, and the evaporation rate from the storage container 9 is It becomes easy to maintain.
- the gas to be introduced it is desirable to use a gas that does not react with the deposition material.
- a gas that does not react with the deposition material For example, when the deposition material is lithium, an inert gas such as helium, argon or nitrogen is desirable.
- oxygen is used as a gas, lithium is oxidized, which makes it impossible to deposit metallic lithium.
- the above-mentioned inert gas can also be used when the vapor deposition material is an organic EL material.
- oxygen gas may be introduced into the gap 50.
- a plurality of support protrusions 60 are provided on the inner bottom surface of the heating container 10.
- the storage container 9 When the storage container 9 is inserted into the recess of the heating container 10, the storage container 9 is supported by the support protrusions 60 so that the outer bottom surface of the storage container 9 does not contact with the inner bottom surface of the heating container 10 It is formed.
- the height of the projection may be adjusted according to the size of the gap to be set.
- a spacer may be disposed on the inner bottom surface of the heating vessel 10.
- a groove functioning as the gap 50 may be formed on the inner bottom surface of the heating container 10. Gas can be introduced into the groove formed on the inner bottom surface of the heating container 10 through the gas introduction pipe 11. In this case, the outer bottom surface of the storage container 9 partially contacts the inner bottom surface of the heating container 10.
- the heat generated by the heater 20 is transferred to the heating container 10 by the contact between the heater 20 and the heating container 10, but in another form shown in FIG. 4, in addition to the configuration of FIG. A space in which the heater 20 is housed inside the component 10 and the inner wall surface of the heating container 10 are in communication via one or more communication paths 67.
- the gas introduced into the gap 50 is also introduced into the space accommodating the heater 20 through the communication passage 67. As a result, the amount of conducted heat is increased, and the heat from the heater is more efficiently transferred to the storage container 9.
- a step shape or a tapered shape is provided around the opening of the heating container 10 and the opening of the storage container 9 By supporting the storage container 9, the outer bottom surface of the storage container 9 can also be prevented from contacting the inner bottom surface of the heating container 10.
- the evaporation source 30 may be provided with a suppression structure that suppresses the flow of gas from the gap 50 into the chamber 2.
- the suppression structure may be configured to change the traveling direction of the gas flowing out of the gap 50, or may be configured to reduce the amount of gas flowing out of the gap 50.
- the pressure of the gap 50 can be increased with a small amount of gas introduced. Further, the reduction of the degree of vacuum in the chamber 2 due to the gas introduction into the gap 50 can be avoided.
- some specific examples of the suppression structure will be described.
- the outer wall surface near the opening of the storage container 9 is provided with a rectangular support 61 projecting outward.
- the support portion 61 By mounting the support portion 61 on the upper end surface of the heating container 10 in the vertical direction, the storage container 9 can be supported so that the outer bottom surface of the storage container 9 does not contact the inner bottom surface of the heating container 10.
- the upper end face in the vertical direction of the heating vessel 10 is provided with a rectangular recess corresponding to the size of the support 61 so that the alignment can be performed by the support 61, but the rectangular recess may be omitted. it can.
- a tapered support portion 63 protruding outward is provided on the outer wall surface near the opening of the storage container 9, and a tapered support portion 63 is provided on the upper end surface of the heating container 10 in the vertical direction. And a tapered recess that matches the In this embodiment, alignment when storing the storage container 9 in the heating container 10 can be accurately performed, and a predetermined gap 50 can be reliably ensured on the side surface and the bottom surface of the storage container 9.
- the gap 50 is closed between the storage container 9 and the opening of the heating container 10 and is isolated from the chamber 2 Space has been Therefore, the pressure of the gap 50 can be increased with a small amount of gas introduced.
- the exhaust pump 1 vacuum pump may be overloaded.
- the communication passage 67 in FIGS. 10 and 11 can be omitted.
- a projection 60 is provided on the inner bottom surface of the heating container 10 to support the storage container 9 and a step shape is provided in the opening of the heating container 10 and the opening of the storage container 9
- the gap 50A in the vicinity of the opening is configured to be narrower than the other gaps 50.
- the rectangular protrusion part 65 which protrudes outside is provided in the outer wall surface of opening part vicinity of the storage container 9, the protrusion part 65 is not in contact with the heating container 10.
- FIG. By narrowing the gap 50A in the vicinity of the opening, the diffusion of the gas introduced into the gap 50 is suppressed, and the pressure of the gap 50 is increased with a small amount of gas introduced. The reduction in the degree of vacuum is suppressed.
- the lid 69 is placed on the upper end surface of the heating container 10 and the upper end surface of the storage container 9, and the upper opening of the gap 50 is closed.
- the presence of the lid 69 suppresses the diffusion of gas into the chamber 2 and can increase the pressure of the gap 50 with a small amount of gas introduced, and can prevent the reduction of the degree of vacuum in the chamber 2.
- the lid 69 has a through hole 71 at the center according to the shape of the opening of the storage container 9 so as not to inhibit evaporation of the vapor deposition material from the storage container 9.
- FIG. 12B and 13B show the lower surface of the lid 69.
- FIG. As shown in these figures, it is desirable that a plurality of groove-shaped gas flow paths 70 be provided on the lower surface of the lid 69.
- the gas flow path 70 is formed to guide the gas introduced into the gap 50 to the outside of the storage container 9 (opposite to the opening of the storage container 9). As a result, the release point of the gas introduced into the gap 50 into the chamber 2 can be located away from the opening of the storage container 9.
- the lid 69 may be configured to change the traveling direction of the gas flowing out of the gap 50, or may be configured to reduce the amount of gas flowing out of the gap 50.
- 12A and 13A are views showing a cross section including the gas flow passage 70, the lower surface of the lid 69 and the upper end surface of the heating container 10 are not in contact with each other. However, in the region other than the gas flow channel 70, the lower surface of the lid 69 and the upper end surface of the heating container 10 are in direct contact with each other.
- the length and the number of the gas flow paths 70 can be set in accordance with the gas pressure of the gap 50.
- the shapes of the heating container 10 and the storage container 9 are rectangular in the form of FIGS. 12A and 14 and circular in the form of FIG. 13A when viewed from the upper end surface or the lower surface.
- the rod-shaped heater 20 is embedded in the heating container 10 from the lower side, facing the vertical direction.
- a flange (convex portion) 72 having a shape corresponding to the opening of the storage container 9 is provided.
- the gas is introduced directly around the heater 20.
- the long hole 15 is formed in the heating container 10.
- the heater 20 is removably inserted into the hole 15.
- the diameter of the hole 15 is slightly larger than the diameter of the heater 20, and a gap is formed between the inner peripheral surface of the hole 15 and the outer peripheral surface of the heater 20.
- a gas introduction pipe 14 (gas introduction path) is connected to the hole 15 so as to introduce a gas into the gap.
- the gas introduced into the hole 15 through the gas introduction pipe 14 is also introduced into the gap 50 through the communication passage 67.
- the gas introduction pipe 11 for directly introducing the gas into the gap 50 may be omitted, or the gas introduction pipe 11 and the gas introduction pipe 14 may be used in combination.
- the structure shown in FIGS. 17 to 26 can be applied to the embodiment shown in FIG.
- the transport unit includes first and second rolls 3 and 8 for winding and holding the substrate 4 and a guide unit for guiding the substrate 4.
- the guide portion has transport rollers 5a and 5b and a cooling can 6 so that the substrate 4 passes a region (vapor deposition region) where the deposition material evaporated from the evaporation surface 9S reaches on the cooling can 6
- the transport path of the substrate 4 is defined.
- a length measuring device (not shown) measures the amount of rotation of the conveyance roller (in this case, the conveyance roller 5 a) which is rotated by the conveyance of the substrate 4, and calculates the movement distance of the substrate 4.
- the first and second rolls 3 and 8, the transport rollers 5a and 5b, and the cooling can 6 have a cylindrical shape of, for example, 600 mm in length, and are arranged in the chamber 2 so that their axes are parallel to each other. It is arranged. Only the cross sections parallel to the bottom of these cylinders are shown in FIG.
- any one of the first and second rolls 3 and 8 delivers the substrate 4, and the transport rollers 5 a and 5 b and the cooling can 6 guide the fed substrate 4 along the transport path.
- the other of the first and second rolls 3 and 8 winds the substrate 4.
- the taken-up substrate 4 is further drawn out by the other roll, and transported in the reverse direction along the transport path, as necessary.
- the first and second rolls 3 and 8 in the present embodiment can function as either a unwinding roll or a winding roll depending on the transport direction.
- the desired number of deposition steps can be continuously performed.
- a shielding unit 13 for shielding radiant heat is installed around the heating container 10. Since the heating vessel 10 is heated to a high temperature of, for example, about 1000 ° C., the shielding unit 13 is provided to reduce the temperature rise of the substrate and the vapor deposition apparatus outside the vapor deposition area as much as possible.
- an evaporation source heating step is performed.
- the long substrate 4 is wound around one of the first and second rolls 3 and 8 (here, the first roll 3).
- metal foil such as aluminum foil, copper foil, nickel foil and the like can be used.
- a copper foil having a thickness of 25 ⁇ m is used.
- a vapor deposition material (lithium metal) is accommodated in the storage container 9.
- the gas introduction pipe 11 is connected to an argon gas cylinder or the like installed outside the vapor deposition apparatus 100. In this state, the exhaust pump 1 is used to evacuate the chamber 2.
- argon gas is introduced into the gap 50 while adjusting the flow rate by the mass flow controller 12.
- the flow rate is controlled so that the vacuum gauge 40 has a target pressure.
- control is performed so that the pressure of the vacuum gauge 40 becomes 5 ⁇ 10 ⁇ 3 Pa.
- the cartridge heater which is the heater 20, to start heating the heating container 10. Since the saturation vapor pressure of lithium at 380 ° C. is approximately 5 ⁇ 10 ⁇ 3 Pa, the temperature of the heating vessel 10 is raised to 380 ° C. As the temperature of the heating vessel 10 rises, the flow rate of argon gas is gradually reduced by the mass flow controller 12 so that the pressure of the vacuum gauge is kept constant. The temperature of the gas in the gap 50 reaches a temperature that exceeds the evaporation temperature of the vapor deposition material (lithium metal).
- an evaporation step is performed as a second step. That is, the temperature of the heating vessel 10 is further raised to evaporate the lithium metal in the storage vessel 9 at a predetermined evaporation rate. In the present embodiment, the temperature of the heating vessel 10 is raised to 600.degree.
- the introduction amount of argon gas is 0.5 SLM (standard liter per minute), but in the evaporation source having the structure shown in FIG.
- the quantity is 0.2 SLM. That is, when the gap 50A around the opening of the storage container 9 and the opening of the heating container 10 is narrowed as shown in FIG. 3, the amount of gas leaking from the gap 50A is small, so a small amount of gas is introduced.
- the quantity can achieve a predetermined gas pressure.
- the current value of the heater 20 is 4 A / piece, but in the evaporation source having the structure shown in FIG. 4, the current value of the heater 20 is 3.4 A / Is a book. That is, when the communication passage 67 (passage passage) for passing the gas is provided between the space for housing the heater 20 and the inner wall surface of the heating container 10 as shown in FIG. Since the heat is transmitted to the storage container 9 more efficiently, the heating amount of the heater 20 can be reduced.
- a deposition film forming step is performed. That is, the substrate 4 wound around the first roll 3 is drawn out, passes the cooling can 6, and is conveyed toward the second roll 8.
- the transfer speed of the substrate 4 is 5 m / min.
- the substrate 4 is deposited as it passes through the deposition zone and is then wound up on the second roll 8. The transport of the substrate 4 is stopped when the predetermined length is deposited.
- a storage container removal step is performed. That is, when the substrate 4 having a predetermined length is drawn out in the third step and the deposition is completed, the current supply to the heater 20 is stopped, and the heating of the heating container 10 is stopped. Although the heating container 10 may wait until it reaches room temperature as it is, in order to shorten the cooling time, the valve 25 is opened to introduce the compressed air into the air cooling passage 68 through the compressed air introducing pipe 26. The introduced compressed air is discharged from the compressed air discharge pipe 27 while cooling the heating vessel 10 through the air cooling passage 68. When the temperature of the heating vessel 10 is lowered to room temperature, the storage vessel 9 can be separated and taken out of the heating vessel 10.
- Test example Using the storage container and the heating container shown in FIG. 13A, a test was conducted to demonstrate the temperature increase effect of the storage container due to the gas introduction.
- the storage container and the heating container were installed under vacuum while the storage container did not hold the vapor deposition material, and while the heating container was heated, the temperatures of the storage container and the heating container were measured over time. Furthermore, the temperature difference between the storage container and the heating container was calculated.
- the result of the case where the measurement is performed without introducing the gas into the gap between the storage container and the heating container is shown in FIG. 16A, and the result when the measurement is performed while introducing the gas (test example) Is shown in FIG. 16B and FIG. 16C.
- Heating container (outer cup): Made of SUS405, coefficient of thermal expansion: 10.8 ⁇ 10 -6 , inner dimension of opening for storing storage container: ⁇ 50.4 ⁇ height 70.2 mm
- Storage container (inner cup): Made of SUS304, coefficient of thermal expansion: 17.3 ⁇ 10 -6 , outer dimension: ⁇ 50 ⁇ height 70 mm
- Heater Sakaguchi Electric Heat cartridge heater. Insert 8 bottles into a heating container and use. Heated with AC40V, 6.3A, 250W.
- the vacuum tank containing the storage container and the heating container was evacuated to 5 Pa by a vacuum pump.
- Nitrogen gas was used as the gas introduced into the gap between the storage container and the heating container.
- the gas flow rate was 20 sccm (standard cubic centimeter per minute).
- the time difference between the heating container and the storage container at the start of heating was as small as 50 seconds.
- the temperature of the storage container followed the temperature of the heating container, and the temperature difference between the heating container and the storage container was small. From FIG. 16C, even when the temperature of the storage container reached 575 ° C., the temperature of the heating container was followed.
- heating the storage container can be efficiently performed under vacuum by introducing a gas into the gap between the heating container and the storage container.
- FIG. 7 is sectional drawing which shows typically the vapor deposition apparatus 200 of 2nd embodiment.
- vapor deposition is performed in the vapor deposition area on the cooling can 6 while conveying the sheet-like substrate 4 in the chamber 2, but the storage container 9 and the heating container
- the openings 10 are formed on the sides of both containers.
- the cooling can 6 is disposed in proximity to the opening formed on the side surface. This also enables vapor deposition of the substrate 4 as in the first embodiment.
- FIG. 9 is a partially enlarged view showing the vicinity of a deposition source of the deposition apparatus of FIG. Similar to FIG. 3, by providing a step shape in the opening of the heating container 10 and the opening of the storage container 9, the gap 50 ⁇ / b> A in the vicinity of the opening is made smaller than the other gaps 50.
- FIG. 8 relates to another form, and shows the case where such a step shape is not provided.
- the deposition can be performed on a substrate which has been left standing, or can be performed on a sheet-like substrate which is conveyed linearly.
- the substrate conveyed in a straight line may be a substrate conveyed horizontally or may be a substrate conveyed in an oblique direction.
- the vacuum deposition apparatus 300 includes a vacuum chamber 81, a vacuum pump 82, an unwinding roller 85, conveying rollers 86a to 86d, a can roller 87, a winding roller 88, and an evaporation source 110.
- the evaporation source 110 is disposed at a position facing the can roller 87.
- the substrate 4 is prepared in the unwinding roll 85, and is fed toward the transport roller 86a.
- the substrate 4 is further transported along the transport roller 86 b, the can roller 87, the transport roller 86 c and the transport roller 86 d, and is taken up by the take-up roll 88.
- the unwinding roll 85, the conveying rollers 86a to 86d, the can roller 87, and the winding roll 88 constitute a conveying system for conveying the substrate 4.
- the material 89 evaporated from the evaporation source 110 is deposited on the substrate 4. Thereby, a thin film containing the material 89 is formed on the substrate 4.
- the inside of the vacuum chamber 81 is maintained at a pressure suitable for thin film production by the action of the vacuum pump 82.
- the degree of vacuum inside the vacuum chamber 81 is not particularly limited, and is, for example, in the range of 10 ⁇ 1 to 10 ⁇ 4 Pa.
- the evaporation source 110 includes a heating block 92 and a plurality of rod-like heaters 20, and is configured as a heating unit that heats an object (material 89) in a vacuum.
- the heating block 92 is an evaporation vessel (crucible) having a recess 21 for containing the material 89 to be evaporated.
- the heating block 92 is heated by supplying a current to the heater 20. By heating the heating block 92 with the heater 20, the material 89 contained in the recess 21 can be melted and evaporated.
- the heating block 92 is formed with a plurality of slots 94 and a plurality of gas introduction paths 97.
- the slot 94 is a long hole in which the heater 20 can be housed. Around the recess 21, the slot 94 extends in a direction (typically, the horizontal direction) parallel to one side of the heating block 92 and penetrates the heating block 92 from one side to the other side. . It is not essential that the slot 94 penetrates the heating block 92.
- the slot 94 may be a bottomed hole.
- the heater 20 is removably inserted into the slot 94.
- the gas introduction path 97 is a path for introducing a heat transfer gas into the gap 96 between the slot 94 and the heater 20.
- the gas introduction path 97 opens at the bottom 92 p of the heating block 92 and communicates with the slot 94 inside the heating block 92.
- a gas supply pipe 95 is connected to the bottom 92 p of the heating block 92 so as to supply the heat transfer gas to the gas introduction path 97. As shown in FIG. 17, the gas supply pipe 95 extends from the heating block 92 to the outside of the vacuum chamber 81.
- the heater 20 has an outer diameter smaller than the inner diameter of the slot 94. Therefore, the heater 20 is in contact with the lower half of the slot 94. Thus, a gap 96 is formed on the heater 20.
- the heat transfer gas is supplied to the gas introduction path 97 through the gas supply pipe 95, the heat transfer gas is introduced into the gap 96 through the gas introduction path 97.
- the gap 96 By filling the gap 96 with the heat transfer gas, heat is efficiently transmitted from the heater 20 to the heating block 92 despite being in a vacuum.
- the evaporation source 110 is used to evaporate the thin film material 89 in a vacuum, and the evaporated material 89 is deposited on the substrate 4 (deposition step or heating step). While performing the deposition process, the heat transfer gas is supplied from the outside of the vacuum chamber 81 to the gas introduction path 97 of the evaporation source 110 through the gas supply pipe 95 so that the gap 96 is filled with the heat transfer gas.
- the type of heat transfer gas is not particularly limited. However, when the present invention is applied to the evaporation source 110, a gas that is likely to react with the material to be deposited and a gas that inhibits the production of a high quality thin film should be avoided. In that respect, an inert gas, in particular, a noble gas such as argon can be suitably used as the heat transfer gas.
- the heating block 92 has a plurality of slots 94 formed therein.
- the heater 20 is inserted into each of the plurality of slots 94.
- a plurality of heaters 20 are disposed to surround the recess 21. According to such a configuration, the heating block 92 can be uniformly heated, and thus the material 89 accommodated in the recess 21 can be uniformly heated.
- the number of heaters 20, slots 94, and gas introduction paths 97 is not particularly limited.
- the gas introduction path 97 includes a first path 97a and a second path 97b.
- the first path 97 a is a path for introducing the heat transfer gas into the specific slot 94 from the outside of the heating block 92.
- the second path 97 b is a path connecting the slots 94 with each other.
- the number of gas supply pipes 95 can be smaller than the number of slots 94. This contributes to the simplification of the structure of the heating block 92.
- the heat transfer gas is supplied to the first path 97a of the gas introduction path 97 through one gas supply pipe 95, and is introduced into the gap 96 of the specific slot 94 through the first path 97a.
- the heat transfer gas is also introduced into the gap 96 of another slot 94 through the second path 97b. Therefore, the heat transfer from the heater 20 to the heating block 92 can be promoted with a small amount of heat transfer gas.
- the evaporation source 110 may be designed such that the conductance of the second path 97 b exceeds the leakage conductance of the path from the gap 96 to the space inside the vacuum chamber 81. In this case, the heat transfer gas dissipated inside the vacuum chamber 81 can be reduced, and the heat transfer gas is easily distributed to the plurality of gaps 96 without excess or deficiency.
- the outer diameter of the heater 20 and the inner diameter of the slot 94 allow the heater 20 to be easily pulled out of the slot 94 and to be inserted easily into the slot 94 even after repeated use of the evaporation source 110. As is properly adjusted. For example, when the outer diameter of the heater 20 is in the range of 5 to 15 mm, the value obtained by subtracting the outer diameter of the heater 20 from the inner diameter of the slot 94 (that is, the width of the gap 96) is in the range of 0.05 to 0.5 mm The inner diameter of the slot 94 can be determined to fit within. If the difference between the outer diameter of the heater 20 and the inner diameter of the slot 94 is within such a range, the vacuum can be maintained without overloading the vacuum pump 82.
- the dimensions of the heater 20 and the dimensions of the slot 94 may be adjusted to allow movement of the heater 20 when energized.
- the difference between the outer diameter of the heater 20 and the inner diameter of the slot 94 may be adjusted.
- the difference between the outer diameter and the inner diameter can be calculated from the linear expansion coefficient of the material of the heater 20, the linear expansion coefficient of the material of the heating block 92, and the operating temperature of the heater 20.
- the heater 20 not be compressed in the slot 94 and that no fasteners, such as screws, be used to secure the heater 20 to the heating block 92. According to such a configuration, it is possible to prevent the large force (load or stress) from being applied to the heater 20 due to the thermal expansion at the time of energization. Therefore, the life of the heater 20 is extended.
- the load applied to the heater 20 may be substantially zero except for the supporting force received from the inner circumferential surface of the slot 94.
- the heating block 92 is made of a heat resistant material such as stainless steel, copper, carbon or the like.
- the heating block 92 has the shape of a bowl.
- the shape, size, and the like of the heating block 92 are not particularly limited.
- the heater 20 is composed of a heater body 31, a lead portion 32 and a connection portion 33.
- the shape of the cross section of the heater 20 is not particularly limited, and is typically circular, and may be oval or rectangular. That is, the heater 20 may have a cylindrical, elliptical or prismatic shape.
- the shape of the cross section of the slot 94 is also not particularly limited, and is typically circular, and may be oval or rectangular.
- the heater main body 31 is connected to the lead portion 32 via the connection portion 33.
- the heater main body 31 has a heating element 34, an insulator 35 a and an outer cylinder 36.
- the lead portion 32 has a pair of lead wires 38 and an insulating coating 39.
- the connection portion 33 has an insulator 35 b, an outer cylinder 36 and a pair of heater wire end portions 37.
- a connecting portion 33 is provided between the lead portion 32 and the heater main body 31 so as to electrically connect the lead wire 38 to the heating element 34. Electrical power is supplied to the heating element 34 through the lead wires 38.
- the outer cylinder 36 may be shared by the heater main body 31 and the connection portion 33.
- the heating element 34 is formed, for example, by winding a metal wire such as tungsten, and is covered by the outer cylinder 36.
- An insulator 35 a is filled between the heating element 34 and the outer cylinder 36.
- An insulation coating 39 is provided to cover the lead wires 38.
- the insulation coating 39 is made of glass fiber, ceramic or the like.
- the lead wire 38 is connected to the heater wire end 37 at the connection point 41 of the connection portion 33.
- a conducting portion is formed by the lead wire 38, the heater wire end portion 37, and the connection point 41.
- An insulator 35 b is filled between the current-carrying portion and the outer cylinder 36.
- the connecting portion 33 does not have to have the outer cylinder 36 and the insulator 35 b as long as the conducting portion is insulated.
- the outer cylinder 36 and the insulator 35 b are provided in the connection portion 33, mechanical robustness in the vicinity of the connection point 41 can be enhanced. Therefore, disconnection due to stress concentration can be prevented.
- the outer cylinder 36 of the connection portion 33 has the same outer diameter as the outer diameter of the outer cylinder 36 of the heater portion 31, the handling of the heater 20 is facilitated.
- the connecting portion 33 be located outside the slot 94 so that the temperatures of the connecting point 41 and the lead 38 do not rise too much. Thereby, the life of the heater 20 can be extended.
- the heater 20 shown in FIG. 21 is merely an example. In the present invention, the type of heater is not particularly limited.
- the slot 94 has a large diameter central portion 94a and a small diameter end portion 94b along the length direction.
- the evaporation source 120 according to the first modification differs from the evaporation source 110 described above.
- the central portion 94a of the slot 94 is a portion in communication with the gas introduction path 97 (the first portion 97a or the second portion 97b).
- the end 94 b of the slot 94 is a portion including the opening of the slot 94.
- the heater 20 has an outer diameter smaller than the inner diameter of the slot 94 at the end 94b.
- the gap 96 is relatively wide at the central portion 94a of the slot 94, and the gap 96 is relatively narrow at the end 94b of the slot 94.
- the center of the central portion 94a coincides with the center of the end 94b. Accordingly, the upper gap 96 a is formed above the heater 20, and the lower gap 96 b is formed below the heater 20.
- the gap 96 In order to keep the heat transfer gas in the gap 96, it is effective to make the inner diameter of the slot 94 as small as possible. However, if the inner diameter of the slot 94 is too small, it will be difficult to withdraw and insert the heater 20.
- the gap 96 since the gap 96 is relatively narrow at the end 94 b of the slot 94, the leakage of the heat transfer gas from the gap 96 can be reduced. Further, since the gap 96 is relatively wide at the central portion 94 a of the slot 94, the heater 20 can be easily pulled out of the slot 94 and the heater 20 can be easily inserted in the slot 94.
- the evaporation source 130 according to the second modification differs from the evaporation source 110 described above in that the evaporation source 130 further includes a cylindrical component 98.
- the cylindrical part 98 is provided at the opening of the slot 94 so as to narrow the gap 96.
- the heater 20 is inserted into the slot 94 through the tubular part 98.
- an upper gap 96 a is formed above the heater 20, and a lower gap 96 b is formed below the heater 20.
- the tubular part 98 plays the same role as reducing the inner diameter of the slot 94. The use of such a tubular part 98 facilitates processing for forming the slot 94 in the heating block 92.
- the cylindrical component 98 has the large diameter part 98a, the small diameter part 98b, and the through-hole 98h.
- the large diameter portion 98 a is a portion having an outer diameter larger than the inner diameter of the slot 94.
- the small diameter portion 98 b is a portion having an outer diameter smaller than the inner diameter of the slot 94.
- the large diameter portion 98a and the small diameter portion 98b are integrally formed.
- the through hole 98 h is formed to penetrate the large diameter portion 98 a and the small diameter portion 98 b.
- the through hole 98 h has an inner diameter larger than the outer diameter of the heater 20. According to the tubular part 98 having such a structure, the gap 96 can be narrowed at the end of the slot 94.
- a hook-like part 28 shown in FIG. 24B may be used instead of the cylindrical part 98 shown in FIG. 24A.
- the bowl-shaped part 28 is obtained by bisecting the cylindrical part 98 in a plane including the central axis of the through hole 98 h.
- the hook-like part 28 may be disposed between the heater 20 and the slot 94.
- the evaporation source 140 according to the third modification differs from the evaporation source 110 described above in that the evaporation source 140 further includes a flange 99 for closing the slot 94.
- the flange 99 is disposed at one of the two openings of the slot 94 that is opposite to the side where the lead wire 38 of the heater 20 is located.
- the slot 94 is closed by the flange 99.
- the flange 99 achieves the same effect as the slot 94 is formed by a bottomed hole.
- the flanges 99 be provided in each of the plurality of slots 94.
- a plate-like member having a size capable of covering the plurality of slots 94 collectively can be used as the flange.
- the flange 99 may only be inserted into the heating block 92, may be screwed in, or may be welded to the heating block 92.
- the method of sealing the slot 94 is not particularly limited.
- the heating device may be a substrate heating device 150 that heats the substrate.
- the substrate heating apparatus 150 includes a heating block 51, a plurality of slots 94 and a plurality of heaters 20.
- a plurality of slots 94 and a plurality of gas introduction paths are formed in the heating block 51.
- the heater 20 is inserted into the slot 94.
- a gas supply pipe 95 is connected to the gas introduction path. By supplying a current to the heater 20, the heating block 51 is entirely heated.
- the heating block 51 is made of, for example, a heat-resistant material that can be used for the heating block 92 of the evaporation source 110.
- the upper surface 51p of the heating block 51 is a surface facing the substrate.
- the substrate can be heated by bringing the substrate close to or in contact with the upper surface 51p.
- the upper surface 51p may be subjected to a process for enhancing the heating efficiency of the substrate. As such processing, forming a black coating on the upper surface 51p to increase the emissivity can be mentioned.
- the structure of the heating block 51 is substantially the same as the structure of the heating block 92 described above, except that it has no recess for receiving the material. That is, all the configurations described for the evaporation sources 110, 120, 130 and 140 can be advantageously applied to the substrate heating apparatus 150. Further, the present invention can be applied to a heating device having a movable portion, such as a heating roller which transports a substrate while heating it.
- the heating device of the present invention can be used for various vacuum devices such as a vacuum deposition device, a vacuum processing device, a vacuum metallurgy device, a vacuum chemistry device, a surface analysis device, and a vacuum test device.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Physical Vapour Deposition (AREA)
Abstract
Description
真空中で加熱されるべき被加熱体と、
前記被加熱体から分離可能、かつ自身と前記被加熱体との間に隙間が形成されるように構成された加熱体と
前記隙間に伝熱ガスを導入するためのガス導入経路と、
を備え、
前記被加熱体は、前記伝熱ガスを介して前記加熱体によって加熱される、加熱装置を提供する。
真空中で加熱されるべき被加熱体と、
前記被加熱体から分離可能、かつ自身と前記被加熱体との間に隙間が形成されるように構成された加熱体と
前記隙間に伝熱ガスを導入するためのガス導入経路と、
を備え、
前記被加熱体は、前記伝熱ガスを介して前記加熱体によって加熱される、加熱装置を提供する。
前記被加熱体は、蒸着材料を保持し、かつ蒸発した前記蒸着材料が通過するための開口部を有する貯蔵容器であり、
前記加熱体は、前記貯蔵容器を脱着可能に格納し、前記貯蔵容器内の前記蒸着材料を加熱するためにヒータを有する加熱容器であって、前記貯蔵容器から蒸発した前記蒸着材料が通過するための開口部を有するとともに、前記貯蔵容器を格納したときに前記貯蔵容器の外壁面と前記加熱容器の内壁面とが直接対向することによって前記内壁面と前記外壁面との間に前記隙間が生じるように構成された加熱容器であり、
前記加熱装置は、(i)前記貯蔵容器及び前記加熱容器を収容し、内部で基材上に蒸着するための真空槽と、(ii)前記真空槽内を排気する真空ポンプと、をさらに備えた蒸着装置である、加熱装置を提供する。
蒸着材料を保持し、かつ蒸発した前記蒸着材料が通過するための開口部を有する貯蔵容器と、
前記貯蔵容器を着脱可能に格納し、前記貯蔵容器内の前記蒸着材料を加熱するためにヒータを有する加熱容器であって、前記貯蔵容器から蒸発した前記蒸着材料が通過するための開口部を有するとともに、前記貯蔵容器を格納したときに前記貯蔵容器の外壁面と前記加熱容器の内壁面とが直接対向することによって前記内壁面と前記外壁面との間に前記隙間が生じるように構成された加熱容器と、
前記貯蔵容器及び前記加熱容器を収容し、内部で基材上に蒸着するための真空槽と、
前記真空槽内を排気する真空ポンプと、
を備えた、蒸着装置を提供する。
蒸着材料を保持し、かつ蒸発した前記蒸着材料が通過するための開口部を有する貯蔵容器と、
前記貯蔵容器を脱着可能に格納し、前記貯蔵容器内の前記蒸着材料を加熱するためにヒータを有する加熱容器であって、前記貯蔵容器から蒸発した前記蒸着材料が通過するための開口部を有するとともに、前記貯蔵容器を格納したときに前記貯蔵容器の外壁面と前記加熱容器の内壁面とが直接対向することによって前記内壁面と前記外壁面との間に隙間が生じるように構成された加熱容器と、
前記隙間に伝熱ガスを導入するためのガス導入手段と、
前記貯蔵容器及び前記加熱容器を収容し、内部で基材上に蒸着するための真空槽と、
前記真空槽内を排気する真空ポンプと、を有する、蒸着装置を使用して、真空中で前記基材上に蒸着を行なう蒸着方法であって、
前記隙間に伝熱ガスを導入しつつ、前記ヒータにより前記貯蔵容器内の前記蒸着材料を加熱することで、前記貯蔵容器から前記蒸着材料を蒸発させる工程を含む、薄膜製造方法を提供する。
前記被加熱体は、真空中で物体を加熱する加熱ブロックであり、
前記加熱体は、前記加熱ブロックに形成されたスロットに着脱可能に差し込まれた棒状のヒータであり、
前記スロットと前記ヒータとの間に前記隙間が形成されており、
前記ガス導入経路は、前記隙間に伝熱ガスを導入するように前記加熱ブロックに形成されている、加熱装置を提供する。
真空中で物体を加熱する加熱ブロックと、
前記加熱ブロックに形成されたスロットと、
前記スロットに着脱可能に差し込まれた棒状のヒータと、
前記加熱ブロックに形成され、前記スロットと前記ヒータとの間の隙間に伝熱ガスを導入するガス導入経路と、
を備えた、加熱装置を提供する。
第一実施形態は、チャンバー内においてシート状の基板を搬送しながら、冷却キャン上の蒸着領域で蒸着を行う形態である。
図1は、第一実施形態の蒸着装置を模式的に示す断面図であり、図2は、図1の蒸着装置の蒸着源付近を拡大して示す部分拡大図である。
次に、蒸着装置100の動作を説明する。ここでは、蒸着装置100を用いて、基板4の表面にリチウム金属膜を形成する場合を例に説明するが、これに限定されない。
図13Aで示した貯蔵容器と加熱容器を用いてガス導入による貯蔵容器の昇温効果を実証する試験を行なった。
貯蔵容器(内カップ):SUS304製、熱膨張係数:17.3×10-6、外寸法:φ50×高さ70mm
ヒータ:坂口電熱製カートリッジヒータ。8本を加熱容器に挿入して使用。AC40V、6.3A、250Wで加熱。
図7は、第二実施形態の蒸着装置200を模式的に示す断面図である。第二実施形態も、第一実施形態と同様、チャンバー2内において、シート状の基板4を搬送しながら、冷却キャン6上の蒸着領域で蒸着を行なう形態であるが、貯蔵容器9及び加熱容器10の開口部は、両容器の側面に形成されている。この側面に形成された開口部に近接するよう、冷却キャン6は配置されている。これによっても、第一実施形態と同様に基板4の蒸着が可能である。
図17に示すように、真空蒸着装置300は、真空槽81、真空ポンプ82、巻き出しロール85、搬送ローラ86a~86d、キャンローラ87、巻き取りロール88及び蒸発源110を備えている。蒸発源110は、キャンローラ87に向かい合う位置に配置されている。基板4は、巻き出しロール85に準備されており、搬送ローラ86aに向かって送り出される。基板4は、さらに、搬送ローラ86b、キャンローラ87、搬送ローラ86c及び搬送ローラ86dに沿って搬送され、巻き取りロール88に巻き取られる。巻き出しロール85、搬送ローラ86a~86d、キャンローラ87及び巻き取りロール88は、基板4を搬送する搬送系を構成している。
図22に示すように、変形例1に係る蒸発源120において、スロット94は、長さ方向に沿って大径の中央部94aと小径の端部94bとを有する。この点に関して、変形例1に係る蒸発源120は、先に説明した蒸発源110と異なる。
図23に示すように、変形例2に係る蒸発源130は、筒状部品98をさらに備えている点で、先に説明した蒸発源110と異なる。
図25に示すように、変形例3に係る蒸発源140は、スロット94を閉じるためのフランジ99をさらに備えている点で、先に説明した蒸発源110と異なる。
本発明は、蒸発源以外の加熱装置にも適用されうる。図26に示すように、加熱装置は、基板を加熱する基板加熱装置150であってもよい。基板加熱装置150は、加熱ブロック51、複数のスロット94及び複数のヒータ20を備えている。加熱ブロック51に複数のスロット94及び複数のガス導入経路(図示省略)が形成されている。スロット94にヒータ20が差し込まれている。ガス導入経路にガス供給管95が接続されている。ヒータ20に電流を流すことによって加熱ブロック51が全体的に加熱される。
Claims (25)
- 真空中で加熱されるべき被加熱体と、
前記被加熱体から分離可能、かつ自身と前記被加熱体との間に隙間が形成されるように構成された加熱体と
前記隙間に伝熱ガスを導入するためのガス導入経路と、
を備え、
前記被加熱体は、前記伝熱ガスを介して前記加熱体によって加熱される、加熱装置。 - 前記被加熱体は、蒸着材料を保持し、かつ蒸発した前記蒸着材料が通過するための開口部を有する貯蔵容器であり、
前記加熱体は、前記貯蔵容器を着脱可能に格納し、前記貯蔵容器内の前記蒸着材料を加熱するためにヒータを有する加熱容器であって、前記貯蔵容器から蒸発した前記蒸着材料が通過するための開口部を有するとともに、前記貯蔵容器を格納したときに前記貯蔵容器の外壁面と前記加熱容器の内壁面とが直接対向することによって前記内壁面と前記外壁面との間に前記隙間が生じるように構成された加熱容器であり、
前記加熱装置は、(i)前記貯蔵容器及び前記加熱容器を収容し、内部で基材上に蒸着するための真空槽と、(ii)前記真空槽内を排気する真空ポンプと、をさらに備えた蒸着装置である、請求項1に記載の加熱装置。 - 前記隙間は、幅が0.5mm以下である、請求項2に記載の加熱装置。
- 前記伝熱ガスが前記隙間から前記真空槽の中に流出することを抑制する抑制構造をさらに備えた、請求項2に記載の加熱装置。
- 前記抑制構造は、前記隙間から流出する前記伝熱ガスの進行方向を変えるように構成されている、又は、前記隙間から流出する前記伝熱ガスの量を低減するように構成されている、請求項4に記載の加熱装置。
- 前記抑制構造は、前記貯蔵容器の前記開口部、及び、前記加熱容器の前記開口部の周囲に設けられた段差構造、又は、テーパー構造である、請求項4に記載の加熱装置。
- 前記段差構造、又は、前記テーパー構造を設けることにより、前記貯蔵容器の前記開口部と前記加熱容器の前記開口部の周囲における前記隙間が、前記開口部の周囲以外の前記隙間よりも狭くなるように形成されている、請求項6に記載の加熱装置。
- 前記加熱容器の熱膨張係数が、前記貯蔵容器の熱膨張係数より小さい、請求項2に記載の加熱装置。
- 前記ヒータを有する前記加熱容器内部の空間と、前記加熱容器の内壁面との間に、前記伝熱ガスを通過させるための通過路、をさらに備えた、請求項2に記載の加熱装置。
- 前記隙間が、前記貯蔵容器の前記開口部と前記加熱容器の前記開口部において、閉鎖されている、請求項2に記載の加熱装置。
- 前記隙間の開口部の上に、蓋体が載置されている、請求項2に記載の加熱装置。
- 前記蓋体の下面に、前記隙間に導入された前記伝熱ガスを通過させるガス流路が形成されている、請求項11に記載の加熱装置。
- 蒸着材料を保持し、かつ蒸発した前記蒸着材料が通過するための開口部を有する貯蔵容器と、
前記貯蔵容器を着脱可能に格納し、前記貯蔵容器内の前記蒸着材料を加熱するためにヒータを有する加熱容器であって、前記貯蔵容器から蒸発した前記蒸着材料が通過するための開口部を有するとともに、前記貯蔵容器を格納したときに前記貯蔵容器の外壁面と前記加熱容器の内壁面とが直接対向することによって前記内壁面と前記外壁面との間に隙間が生じるように構成された加熱容器と、
前記隙間に伝熱ガスを導入するためのガス導入手段と、
前記貯蔵容器及び前記加熱容器を収容し、内部で基材上に蒸着するための真空槽と、
前記真空槽内を排気する真空ポンプと、を有する、蒸着装置を使用して、真空中で前記基材上に蒸着を行なう蒸着方法であって、
前記隙間に伝熱ガスを導入しつつ、前記ヒータにより前記貯蔵容器内の前記蒸着材料を加熱することで、前記貯蔵容器から前記蒸着材料を蒸発させる工程を含む、薄膜製造方法。 - 前記伝熱ガスの導入量は、前記真空槽内の圧力に応じて制御される、請求項13に記載の薄膜製造方法。
- 前記蒸着材料がリチウムであり、前記伝熱ガスが不活性ガスである、請求項13に記載の薄膜製造方法。
- 前記被加熱体は、真空中で物体を加熱する加熱ブロックであり、
前記加熱体は、前記加熱ブロックに形成されたスロットに着脱可能に差し込まれた棒状のヒータであり、
前記スロットと前記ヒータとの間に前記隙間が形成されており、
前記ガス導入経路は、前記隙間に伝熱ガスを導入するように前記加熱ブロックに形成されている、請求項1に記載の加熱装置。 - 前記加熱ブロックには、複数の前記スロットが形成されており、
複数の前記スロットのそれぞれに前記ヒータが差し込まれており、
前記ガス導入経路は、前記加熱ブロックの外部から前記スロットに前記伝熱ガスを導入する第一経路と、前記スロット同士を互いに連通する第二経路とを含む、請求項16に記載の加熱装置。 - 前記スロットの長さ方向の中央部で前記隙間が相対的に広く、前記スロットの長さ方向の端部で前記隙間が相対的に狭い、請求項16に記載の加熱装置。
- 前記ヒータが、発熱体を有するヒータ本体と、前記発熱体に電力を供給するように前記ヒータ本体の前記発熱体に電気的に接続されたリード線とを有し、
前記リード線が位置する側とは反対側において、前記スロットが閉じられている、請求項16に記載の加熱装置。 - 通電時に前記ヒータの動きが許容されるように、前記ヒータの寸法及び前記スロットの寸法が調節されている、請求項16に記載の加熱装置。
- 前記ヒータが、発熱体を有するヒータ本体と、前記発熱体に電力を供給するためのリード線を有するリード部と、前記リード線を前記発熱体に電気的に接続するように前記リード部と前記ヒータ本体との間に設けられた接続部とを有し、
前記接続部が前記スロットの外に位置している、請求項16に記載の加熱装置。 - 前記加熱装置が蒸発源であり、
前記加熱ブロックが、蒸発させるべき材料としての前記物体を収容する凹部を有する蒸発容器である、請求項16に記載の加熱装置。 - 前記加熱装置が基板を加熱する基板加熱装置である、請求項16に記載の加熱装置。
- 請求項16に記載の加熱装置を使用して真空中で前記物体を加熱する工程と、
前記加熱工程を実施しながら、真空の外部から前記加熱装置に前記伝熱ガスを供給する工程と、
を含む、真空加熱方法。 - 請求項16に記載の加熱装置を使用し、前記物体としての薄膜の材料を真空中で蒸発させ、蒸発した材料を基板上に堆積させる工程と、
前記堆積工程を実施しながら、真空の外部から前記加熱装置に前記伝熱ガスを供給する工程と、
を含む、薄膜製造方法。
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR1020137004819A KR101489099B1 (ko) | 2011-06-29 | 2012-06-28 | 가열 장치, 진공 가열 방법 및 박막 제조 방법 |
CN201280002579.4A CN103080366B (zh) | 2011-06-29 | 2012-06-28 | 加热装置、真空加热方法和薄膜制造方法 |
JP2013522453A JP5584362B2 (ja) | 2011-06-29 | 2012-06-28 | 加熱装置、真空加熱方法及び薄膜製造方法 |
US13/820,141 US20130189424A1 (en) | 2011-06-29 | 2012-06-28 | Heating apparatus, vacuum-heating method and method for manufacturing thin film |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2011144561 | 2011-06-29 | ||
JP2011-144561 | 2011-06-29 | ||
JP2011244664 | 2011-11-08 | ||
JP2011-244664 | 2011-11-08 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2013001827A1 true WO2013001827A1 (ja) | 2013-01-03 |
Family
ID=47423744
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2012/004212 WO2013001827A1 (ja) | 2011-06-29 | 2012-06-28 | 加熱装置、真空加熱方法及び薄膜製造方法 |
Country Status (5)
Country | Link |
---|---|
US (1) | US20130189424A1 (ja) |
JP (1) | JP5584362B2 (ja) |
KR (1) | KR101489099B1 (ja) |
CN (1) | CN103080366B (ja) |
WO (1) | WO2013001827A1 (ja) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2016030839A (ja) * | 2014-07-28 | 2016-03-07 | 株式会社Joled | 蒸着装置および蒸発源 |
KR20180098668A (ko) * | 2015-12-31 | 2018-09-04 | 차이나 트라이엄프 인터내셔널 엔지니어링 컴퍼니 리미티드 | 재료를 용납 및 가열하는 도가니 및 도가니와 히터 구성을 포함하는 시스템 |
CN109297081A (zh) * | 2018-10-19 | 2019-02-01 | 江苏长青艾德利装饰材料有限公司 | 墙地暖发热模块及集成墙地暖*** |
JPWO2021153104A1 (ja) * | 2020-01-28 | 2021-08-05 | ||
JP2022084168A (ja) * | 2020-11-26 | 2022-06-07 | プライムプラネットエナジー&ソリューションズ株式会社 | 電極積層体、電池、および電極積層体の製造方法 |
Families Citing this family (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR101854934B1 (ko) * | 2013-07-15 | 2018-06-20 | 주식회사 엘지화학 | 연료전지의 연료극 형성 장치 및 방법, 이에 의해 제조된 고체산화물 연료전지의 연료극 및 이를 포함하는 고체산화물 연료전지 |
CN106929802B (zh) * | 2015-12-31 | 2021-06-04 | 中国建材国际工程集团有限公司 | 用于加热坩埚的加热器设备和用于蒸发或升华材料的*** |
KR101837997B1 (ko) * | 2016-07-04 | 2018-03-15 | 재단법인 포항산업과학연구원 | 박막 제조 장치 및 이를 이용한 리튬 이차전지용 음극의 제조방법 |
JP6205028B1 (ja) * | 2016-07-22 | 2017-09-27 | マシン・テクノロジー株式会社 | 蒸発装置およびそれに用いる固定具 |
CN106868456B (zh) * | 2017-03-21 | 2019-03-12 | 京东方科技集团股份有限公司 | 蒸发源和蒸镀设备 |
CN106864146A (zh) * | 2017-03-30 | 2017-06-20 | 晋江市曙光机械有限公司 | 一种金纸的锡箔烫印机 |
WO2018199184A1 (ja) * | 2017-04-26 | 2018-11-01 | 株式会社アルバック | 蒸発源及び成膜装置 |
CN111074210A (zh) * | 2018-10-18 | 2020-04-28 | 大永真空科技股份有限公司 | 适用于纱线镀膜的腔体 |
KR102319130B1 (ko) * | 2020-03-11 | 2021-10-29 | 티오에스주식회사 | 가변 온도조절 장치를 구비한 금속-산화물 전자빔 증발원 |
US20220228250A1 (en) * | 2021-01-15 | 2022-07-21 | Phoenix Silicon International Corp. | Crucible and vapor deposition apparatus |
CN115369361B (zh) * | 2021-08-26 | 2023-12-22 | 广东聚华印刷显示技术有限公司 | 蒸镀坩埚、蒸镀设备以及蒸镀方法 |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS62180067A (ja) * | 1986-02-03 | 1987-08-07 | Matsushita Electric Ind Co Ltd | 電子ビ−ム蒸着装置および電子ビ−ム蒸着方法 |
JPH0293063A (ja) * | 1988-09-30 | 1990-04-03 | Mitsubishi Heavy Ind Ltd | 真空蒸発装置用るつぼ |
JPH09143694A (ja) * | 1995-11-14 | 1997-06-03 | Ishikawajima Harima Heavy Ind Co Ltd | 真空蒸着装置のルツボ加熱方法 |
US6384367B1 (en) * | 1999-05-04 | 2002-05-07 | Satis Vacuum Industries Vertriebs-Ag | Electron beam vaporizer for vacuum coating systems |
US20040200416A1 (en) * | 2003-04-09 | 2004-10-14 | Heiko Schuler | Effusion cell with improved temperature control of the crucible |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6991684B2 (en) * | 2000-09-29 | 2006-01-31 | Tokyo Electron Limited | Heat-treating apparatus and heat-treating method |
CN201158700Y (zh) * | 2008-01-17 | 2008-12-03 | 北儒精密股份有限公司 | 真空设备的加热装置 |
-
2012
- 2012-06-28 WO PCT/JP2012/004212 patent/WO2013001827A1/ja active Application Filing
- 2012-06-28 CN CN201280002579.4A patent/CN103080366B/zh not_active Expired - Fee Related
- 2012-06-28 US US13/820,141 patent/US20130189424A1/en not_active Abandoned
- 2012-06-28 JP JP2013522453A patent/JP5584362B2/ja not_active Expired - Fee Related
- 2012-06-28 KR KR1020137004819A patent/KR101489099B1/ko not_active IP Right Cessation
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS62180067A (ja) * | 1986-02-03 | 1987-08-07 | Matsushita Electric Ind Co Ltd | 電子ビ−ム蒸着装置および電子ビ−ム蒸着方法 |
JPH0293063A (ja) * | 1988-09-30 | 1990-04-03 | Mitsubishi Heavy Ind Ltd | 真空蒸発装置用るつぼ |
JPH09143694A (ja) * | 1995-11-14 | 1997-06-03 | Ishikawajima Harima Heavy Ind Co Ltd | 真空蒸着装置のルツボ加熱方法 |
US6384367B1 (en) * | 1999-05-04 | 2002-05-07 | Satis Vacuum Industries Vertriebs-Ag | Electron beam vaporizer for vacuum coating systems |
US20040200416A1 (en) * | 2003-04-09 | 2004-10-14 | Heiko Schuler | Effusion cell with improved temperature control of the crucible |
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2016030839A (ja) * | 2014-07-28 | 2016-03-07 | 株式会社Joled | 蒸着装置および蒸発源 |
KR20180098668A (ko) * | 2015-12-31 | 2018-09-04 | 차이나 트라이엄프 인터내셔널 엔지니어링 컴퍼니 리미티드 | 재료를 용납 및 가열하는 도가니 및 도가니와 히터 구성을 포함하는 시스템 |
JP2019506536A (ja) * | 2015-12-31 | 2019-03-07 | チャイナ トライアンフ インターナショナル エンジニアリング カンパニー リミテッドChina Triumph International Engineering Co.,Ltd. | 材料を収容・加熱する坩堝及び坩堝と加熱器セットを含むシステム |
KR102138990B1 (ko) | 2015-12-31 | 2020-07-29 | 차이나 트라이엄프 인터내셔널 엔지니어링 컴퍼니 리미티드 | 재료를 용납 및 가열하는 도가니 및 도가니와 히터 구성을 포함하는 시스템 |
CN109297081A (zh) * | 2018-10-19 | 2019-02-01 | 江苏长青艾德利装饰材料有限公司 | 墙地暖发热模块及集成墙地暖*** |
CN109297081B (zh) * | 2018-10-19 | 2023-09-01 | 江苏长青艾德利装饰材料有限公司 | 墙地暖发热模块及集成墙地暖*** |
JPWO2021153104A1 (ja) * | 2020-01-28 | 2021-08-05 | ||
JP7113964B2 (ja) | 2020-01-28 | 2022-08-05 | 株式会社アルバック | 蒸着源、蒸着装置 |
JP2022084168A (ja) * | 2020-11-26 | 2022-06-07 | プライムプラネットエナジー&ソリューションズ株式会社 | 電極積層体、電池、および電極積層体の製造方法 |
JP7213225B2 (ja) | 2020-11-26 | 2023-01-26 | プライムプラネットエナジー&ソリューションズ株式会社 | 電極積層体、電池、および電極積層体の製造方法 |
Also Published As
Publication number | Publication date |
---|---|
CN103080366B (zh) | 2014-12-24 |
CN103080366A (zh) | 2013-05-01 |
JPWO2013001827A1 (ja) | 2015-02-23 |
US20130189424A1 (en) | 2013-07-25 |
KR20130032912A (ko) | 2013-04-02 |
JP5584362B2 (ja) | 2014-09-03 |
KR101489099B1 (ko) | 2015-02-02 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
WO2013001827A1 (ja) | 加熱装置、真空加熱方法及び薄膜製造方法 | |
US8877291B2 (en) | Method of manufacturing thin film which suppresses unnecessary scattering and deposition of a source material | |
US8865258B2 (en) | Method of manufacturing thin film which suppresses unnecessary scattering and deposition of a source material | |
US20130112670A1 (en) | Heat treatment apparatus | |
KR102137181B1 (ko) | 증착 배열체, 증착 장치 및 그의 동작 방법들 | |
KR20210019131A (ko) | 증발기, 증착 배열체, 증착 장치 및 이들의 작동 방법들 | |
US10837098B2 (en) | Method and coating arrangement | |
JP5058396B1 (ja) | 薄膜の製造方法及び製造装置 | |
JP2013249505A (ja) | 成膜装置及び成膜方法 | |
TWI527925B (zh) | 用於鍍膜基板的結構配置 | |
JP2007063615A (ja) | リチウムまたはリチウム合金薄膜の形成方法 | |
KR101224529B1 (ko) | 열처리장치 | |
JP4056680B2 (ja) | 成膜装置及び方法 | |
JP3580101B2 (ja) | リチウムイオン電池負極材料の製造方法及び装置 | |
US20210381097A1 (en) | Vapor deposition apparatus and method for coating a substrate in a vacuum chamber | |
JP6132055B2 (ja) | グラフェン膜の製造方法 | |
KR101539624B1 (ko) | 증착 물질 연속 공급장치 및 이를 이용한 하향식 내지문 코팅 증착 장치와 인라인 설비 | |
JP2019214033A (ja) | 原料をマイクロ波表面波プラズマで処理して原料と異なる生成物を得る製造装置及び製造方法 | |
TWI839614B (zh) | 液體材料驟蒸發坩堝、蒸氣沉積設備及用於塗覆真空腔室內的基板的方法 | |
JP4683418B2 (ja) | プラズマcvd装置 | |
JP2022119452A (ja) | 処理装置 | |
JP2010189683A (ja) | 成膜方法及び成膜装置 | |
TW202314014A (zh) | 用於物理氣相沉積腹板塗覆的封閉耦接擴散器 | |
JP2008294154A (ja) | Cvd装置 | |
JP2006299353A (ja) | 成膜装置及び成膜方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
WWE | Wipo information: entry into national phase |
Ref document number: 201280002579.4 Country of ref document: CN |
|
ENP | Entry into the national phase |
Ref document number: 2013522453 Country of ref document: JP Kind code of ref document: A |
|
ENP | Entry into the national phase |
Ref document number: 20137004819 Country of ref document: KR Kind code of ref document: A |
|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 12805202 Country of ref document: EP Kind code of ref document: A1 |
|
WWE | Wipo information: entry into national phase |
Ref document number: 13820141 Country of ref document: US |
|
NENP | Non-entry into the national phase |
Ref country code: DE |
|
122 | Ep: pct application non-entry in european phase |
Ref document number: 12805202 Country of ref document: EP Kind code of ref document: A1 |