JP6185751B2 - Vacuum suction method, vacuum processing apparatus, and sublimation pump - Google Patents

Description

  The present invention relates to a vacuum suction method, a vacuum processing apparatus, and a sublimation pump for evacuating a vacuum processing chamber when processing the surface of a workpiece such as a substrate.

  2. Description of the Related Art Conventionally, there are many apparatuses that perform work by evacuating a processing chamber, such as a sputtering apparatus, a plasma CVD apparatus, and an ion implantation apparatus. In these apparatuses, taking a sputtering apparatus as an example, the vacuum processing chamber is vacuum-sucked before or while sputtering is performed on the surface of the substrate from the target. In these apparatuses, a component generated by sputtering adheres to the processing chamber, and a vacuum atmosphere originally required by a gas released from the attached film and a gas generated by the heating action of plasma discharge or sputtering is generated. May deteriorate. For this reason, it is known that in a sputtering apparatus or the like, it takes time to vacuum the inside of the processing chamber and reach a predetermined degree of vacuum.

  Moreover, as a device for shortening the time until the vacuum state is reached, for example, a semiconductor device manufacturing chamber device has been proposed (see Patent Document 1). The semiconductor device manufacturing chamber apparatus has a configuration in which a mounting table is installed at a central portion of the bottom surface inside the chamber, and a dome-shaped shield that covers the top of the mounting table is provided in the upper part of the chamber, A heating source provided between the outer surface of the shield and the wall of the chamber, and temperature control means for controlling the heating source are provided. The semiconductor device manufacturing chamber apparatus heats the shield and the wall of the chamber with a heating source so that the chamber wall and the shield heated by the heating source are constantly maintained at a predetermined temperature. It is comprised so that it may control with a control means.

  Furthermore, a sublimation pump that evacuates the vacuum processing chamber is known (see Non-Patent Document 1). This pump heats the titanium evaporation filament to below the melting point and sublimates it in a vacuum, thereby creating a titanium film in the vapor phase on the wall surface in the pump, and using the titanium getter action, Adsorption is performed to promote the exhaust action. Moreover, even if the adsorption surface of the wall surface in the pump is saturated with gas molecules, the sublimation pump can secure the adsorption surface by forming a titanium film on the surface.

Japanese Patent Application Laid-Open No. 09-190977

ULVAC website, as of November 20, 2012 (http://www.shinku-pump.com/vacuumpump/sublimation/)

  However, in the above-described apparatus, even if the temperature in the chamber can be kept constant, depending on the raw materials used in the process of forming a film on the substrate in the chamber and the components of the target, the inside of the chamber is vacuumed. It took a long time. In addition, since conventional sublimation pumps use titanium as the main component of the filament that is used for vacuum suction, it is difficult to obtain because of the scarce value and price of titanium. Since there is a problem with instability such as the number 0.46 (foreign product)), improvement has been desired.

  The present invention has been made in view of such points, and it is possible to evacuate the vacuum processing chamber in a short time regardless of the raw material to be processed, and to obtain a material that can be easily obtained for evacuation. It is an object of the present invention to provide a vacuum suction method, a vacuum suction device, and a sublimation pump that can be used.

In order to solve the above-described problem, a vacuum suction method is a preliminary that communicates a Si-based material in a solid state, which is one of Si, Si alloy, Si compound, and Si mixture, adjacent to the vacuum processing chamber or the vacuum processing chamber. was placed in a room, said vacuum processing chamber, or, in the preliminary chamber, and directly or indirectly a gas phase the Si material from the solid state, Si on at least a portion of the vacuum processing chamber or pre-chamber A system deposition film was deposited to evacuate the vacuum processing chamber or the vacuum processing chamber and the preliminary chamber. The Si-based material is a wire-like Si-based filament, and the preliminary chamber is a filament storage chamber for storing the Si-based filament, and is heated and sublimated at a temperature equal to or lower than the melting point of the Si-based filament. The Si-based deposition film may be deposited and formed on at least a part of the filament storage chamber.

According to such a procedure, in the vacuum suction method, in addition to vacuum suction in the vacuum processing chamber by the vacuum pump by heating and sublimating the Si-based filament and depositing a Si-based deposition film at a position facing the Si-based filament, Adsorption action by Si dangling bonds of the Si-based deposited film works, and gases unnecessary for vacuum are rapidly removed.

In addition, the vacuum suction method is to install a Si-based material in a solid phase which is any one of Si, Si alloy, Si compound, and Si mixture in a vacuum processing chamber or a preliminary chamber communicating adjacent to the vacuum processing chamber, In the vacuum processing chamber or the preliminary chamber, the Si-based material is directly or indirectly changed from a solid phase to a gas phase, and a Si-based deposition film is deposited in at least a part of the vacuum processing chamber or the preliminary chamber. Let the vacuum processing chamber or the vacuum processing chamber and the preliminary chamber be evacuated, and the Si-based material is a Si-based heated material that is any of powder, granules, sheets, or pellets, The Si-based material to be heated is placed in a storage container such as a boat or a crucible and installed in one of the vacuum processing chamber or the preliminary chamber. The heating means provided in the vacuum processing chamber or the preliminary chamber is used in the storage container. S The system was heated material is melted by heating to the melting point or more and evaporated, may be formed by depositing at least a portion or the Si-based deposited film on at least a portion of the preliminary chamber of the vacuum processing chamber.

According to such a procedure, in the vacuum suction method, when processing the surface of a workpiece such as a substrate in a vacuum processing chamber, the Si-based material is heated by, for example, an electron gun, a crucible, or a boat, and is sputtered by applying a voltage. Thus, the Si-based deposition film is deposited or deposited in at least a part of the vacuum processing chamber or the preliminary chamber from the solid phase state to the gas phase state, and then vacuumed by a vacuum pump. As a result, in this vacuum suction method, component molecules that are unnecessary for the vacuum mixed in the atmosphere in the vacuum processing chamber due to the adsorption action of the dangling bonds of the Si-based deposited film are adsorbed to the Si-based deposited film, and the vacuum The state can be realized earlier than in the past. According to such a procedure, in the vacuum suction method, a shutter or a boat, a crucible, or the like is evaporated in the vicinity of the work so that the melted and evaporated Si-based material does not accumulate on the work processed in the vacuum processing chamber. A shielding plate is installed in the vicinity of the source, and the Si-based material to be heated is melted and evaporated to form a Si-based deposition film in at least one of the vacuum processing chamber and the preliminary chamber. In addition to the vacuum suction in the vacuum processing chamber by the vacuum pump, the adsorption action by the Si dangling bonds of the Si-based deposited film works and the gas unnecessary for the vacuum is rapidly removed.

In the vacuum processing method described above, the gas that becomes the inert gas, the mixed gas of the inert gas and the reactive gas, or the reactive gas in the vacuum processing chamber, or in the vacuum processing chamber and the spare chamber. The Si-based film may be deposited in an atmosphere or a vacuum atmosphere.
According to such a procedure, when the vacuum inside the vacuum processing chamber is evacuated by a vacuum pump while depositing a Si-based deposition film, the set vacuum state can be reached quickly in a vacuum state, and the atmosphere in the gas atmosphere Even after the gas introduction is stopped and the gas is exhausted, the set vacuum state can be reached quickly.

In order to solve the above-mentioned problem, the vacuum processing apparatus performs work processing in an inert gas, a mixed gas of an inert gas and a reactive gas, or a gas atmosphere that becomes a reactive gas, or in a vacuum atmosphere. A vacuum processing apparatus comprising: a vacuum processing chamber that communicates with the vacuum processing chamber; and a vacuum chamber that is connected to the vacuum processing chamber and evacuates the vacuum processing chamber. An installation part for installing a Si-based material in a solid state that is any one of Si, Si alloy, Si compound, and Si mixture in a room or the spare room, and a Si-based material installed in the installation part in a solid state A vapor phase means for directly or indirectly bringing the Si-based deposition film into the vacuum processing chamber or at least a part of the preliminary chamber by the vapor phase means. Or after depositing the Si-based deposition film in the gas atmosphere, the vacuum pump is operated, the Si-based material is a wire-like Si-based filament, and the preliminary chamber is the Si-based filament A filament storage chamber for storing filaments, which is heated to sublimate below the melting point of the Si-based filament to be in a gas phase state, and is formed by depositing the Si-based deposition film on at least a part of the filament storage chamber. It was configured as follows.

According to this configuration, the vacuum processing apparatus converts the Si-based material installed in the installation unit from the solid phase state to the gas phase state by the vapor phase means, and forms the Si-based deposition film in at least a part of the vacuum processing chamber or the preliminary chamber. To do. In addition to the vacuum pump, the vacuum processing apparatus can rapidly remove gas unnecessary for vacuum by the Si-based deposited film. Further, the vacuum processing apparatus heats and sublimates the Si-based filament and deposits the Si-based deposition film at a position facing the Si-based filament, so that in addition to vacuum suction in the vacuum processing chamber by a vacuum pump, the Si-based deposition film Adsorption action by the Si dangling bond works and gas unnecessary for vacuum is rapidly removed.

Further, the vacuum processing apparatus includes an inert gas, a mixed gas of an inert gas and a reactive gas, a gas atmosphere that becomes a reactive gas, or a vacuum processing chamber that performs workpiece processing in a vacuum atmosphere, A vacuum processing apparatus comprising a preliminary chamber communicating adjacent to a vacuum processing chamber, and a vacuum pump connected to the vacuum processing chamber and evacuating the vacuum processing chamber, wherein the vacuum processing chamber or the preliminary chamber is An installation unit for installing a Si-based material in a solid phase that is any one of Si, Si alloy, Si compound, and Si mixture, and an Si-based material installed in the installation unit directly or indirectly from the solid phase A gas phase means for setting the gas phase state, and depositing the Si-based deposited film in at least a part of the vacuum processing chamber or the preliminary chamber by the gas phase means in the vacuum atmosphere, or After depositing the Si-based deposition film in an atmosphere, the vacuum pump is operated, and the Si-based material is a Si-based material to be heated that is any of powder, granules, sheets, or pellets, A Si-based material to be heated is placed in a storage container such as a boat or a crucible, and is placed in one of the vacuum processing chamber or the preliminary chamber, and Si in the storage container is heated by heating means provided in the vacuum processing chamber or the preliminary chamber. The system heated material is heated to a melting point or higher to be melted and evaporated, and the Si-based deposition film is deposited and formed in at least a part of the vacuum processing chamber or at least a part of the preliminary chamber.
According to this configuration, the vacuum processing apparatus converts the Si-based material installed in the installation unit from the solid phase state to the gas phase state by the vapor phase means, and forms the Si-based deposition film in at least a part of the vacuum processing chamber or the preliminary chamber. To do. In addition to the vacuum pump, the vacuum processing apparatus can rapidly remove gas unnecessary for vacuum by the Si-based deposited film. In addition, the vacuum processing equipment has a shutter in the immediate vicinity of the workpiece or a shielding plate in the vicinity of the evaporation source such as a boat or crucible so that the melted and evaporated Si-based material does not accumulate on the workpiece processed in the vacuum processing chamber. Then, the Si-based material to be heated is melted and evaporated to form a Si-based deposited film in at least one of the vacuum processing chamber and the preliminary chamber. In addition to the vacuum suction in the vacuum processing chamber by the vacuum pump, the adsorption action by the Si dangling bonds of the Si-based deposited film works and the gas unnecessary for the vacuum is rapidly removed.

Furthermore, in order to solve the above-mentioned problem, it is a sublimation pump that performs vacuum suction in a vacuum processing chamber, and is formed from a Si-based material in a solid phase that is any one of Si, Si alloy, Si compound, and Si mixture. A Si-based filament, a support that supports both ends of the Si-based filament, a power source that heats the filament through the support at a melting point or less and sublimates, and an inner peripheral surface that faces the Si-based filament The Si-based filament is sublimated via the power source to form a Si-based deposited film on the inner peripheral surface of the cylindrical body and vacuum suction is performed.
According to such a configuration, the sublimation pump heats and sublimates the Si-based filament by the power source, forms a Si-based deposited film on the inner peripheral surface of the cylindrical body, and forms a Si dangling bond to remove unnecessary gas in the vacuum. It is removed by adsorption action.

According to the present invention, the following excellent effects can be obtained.
In the vacuum suction method, a Si-based deposited film is formed in at least a part of a vacuum processing chamber or a spare chamber with a Si-based material in a gas phase state, and vacuumed by a vacuum pump together, thereby depositing a Si-based material. By the adsorption action by the Si dangling bonds of the deposited film, the gas hindering the vacuum floating in the vacuum processing chamber can be adsorbed and removed, and the exhaust efficiency can be improved.

  In order to perform vacuum suction with a vacuum pump after forming or depositing a Si-based deposition film from a solid-phase state to a gas-phase state by a vapor-phase means, or after depositing a Si-based material installed in the installation unit, With a simple configuration, it is possible to remove the gas that obstructs the vacuum by the adsorption action of the Si-based deposited film by the Si dangling bond, improve the exhaust efficiency, and secure the vacuum state in a short time.

  Since the sublimation pump uses Si-based filaments, it is easy to procure raw materials, and the gas that hinders vacuum is removed by the adsorption action of Si dangling bonds by the Si deposited film, and the vacuum processing chamber is quickly opened. It is possible to create a vacuum.

It is a schematic diagram which shows typically the vacuum processing apparatus which concerns on this invention. It is a schematic diagram which shows typically the sublimation pump used for the vacuum processing chamber apparatus which concerns on this invention. It is a flowchart which shows typically the flow about the vacuum processing method which concerns on this invention. (A) is a schematic diagram schematically showing the structure of a Si-based material deposited film in the vacuum suction method according to the present invention, and (b) is a dangling bond to the Si-based material deposited film in the vacuum suction method according to the present invention. It is a schematic diagram which shows typically the state of the adsorption effect by. It is a schematic diagram which shows 2nd Embodiment of the vacuum processing apparatus and vacuum suction method which concern on this invention. 6 is a flowchart schematically showing a flow of a vacuum suction method in the vacuum processing apparatus of FIG. 5 according to the present invention. It is a schematic diagram which shows 3rd Embodiment of the vacuum processing apparatus and vacuum suction method which concern on this invention.

  A vacuum suction method, a vacuum processing apparatus, and a sublimation pump according to the present invention will be described with reference to the drawings. First, a configuration of a vacuum processing apparatus using a sublimation pump and a vacuum suction method will be described.

  As shown in FIG. 1, the vacuum processing apparatus 1 includes a housing 2 that is a processing chamber capable of processing a workpiece W with a vacuum inside, and a holding that holds the workpiece W to be processed in the housing 2. A mechanism 3, a storage container 4 for storing a vapor deposition material Gz to be vapor-deposited on the workpiece W held by the holding mechanism 3, an electron gun 5 which is a vapor phase means for heating the vapor deposition material Gz of the storage container 4, and this A shutter mechanism 6 for controlling the vapor deposition material Gz in the storage container 4 heated by the electron gun 5 to be vapor-deposited and non-vapor-deposited on the work W, and a sublimation pump 10 as an auxiliary pump for creating a vacuum state in the housing 2. And.

  The casing 2 is capable of performing a process such as vapor deposition with the inside being evacuated, and penetrates the vacuum processing chamber 2a, the open / close lid 2b provided on the upper portion of the vacuum processing chamber 2a, and the outer wall of the vacuum processing chamber 2a. And a main vacuum pump Ps connecting portion 2c and an atmosphere gas introducing portion 2d formed through the outer wall of the vacuum processing chamber 2a. In addition, the housing 2 is configured such that the electron gun 5 and the sublimation pump 10 installed in the vacuum processing chamber 2a can be connected to respective power sources. The housing 2 is used as a state in which the inside is evacuated by being sucked by the main vacuum pump Ps and the sublimation pump 10 connected via the connecting portion 2c. In addition, the processing operation is performed on the housing 2 in a state where a predetermined gas atmosphere is provided by the atmospheric gas supplied from the atmospheric gas container Fg connected to the housing 2 via the introduction portion 2d.

The holding mechanism 3 holds the workpiece W to be processed in the housing 2. The holding mechanism 3 only needs to have a configuration capable of holding the workpiece surface to be processed so as to expose the workpiece W, and further has a configuration capable of rotating the workpiece surface in a direction parallel to the horizontal plane. As long as it is provided, the configuration is not limited.
Here, the storage container 4 is made of a heat-resistant container such as a crucible or a boat (a container in which a concave groove is formed from one side of a rectangular parallelepiped), and is made of a material that can withstand the vapor deposition material Gz that is stored and heated. Has been. The storage container 4 is not particularly limited as long as it has a general configuration that is durable even when the evaporation material Gz is melted and evaporated by an electron beam.

  The electron gun 5 melts the vapor deposition material Gz stored in the storage container 4. The electron gun 5 here melts the vapor deposition material Gz by deflecting the irradiation path of the electron beam. As long as the electron gun 5 is configured to melt the vapor deposition material Gz so that the vapor deposition operation can be performed, the electron gun 5 directly irradiates the electron beam without deflecting the electron beam, even if the electron gun 5 is configured to deflect the electron beam. It may be configured.

  The shutter mechanism 6 controls vapor deposition by evaporation from the vapor deposition material Gz stored in the storage container 4. In this shutter mechanism 6, here, a shielding plate is installed between the deposition path between the storage container 4 and the work W, and the shielding plate shields all or a part of the deposition path or moves to the retracted position. Thus, the vapor deposition operation from the vapor deposition material Gz is controlled depending on whether or not the vapor deposition path is shielded. The shutter mechanism 6 is not particularly limited in terms of material, structure, drive mechanism, and the like as long as it can be deposited and blocked.

  The vapor deposition material Gz is a material used for the surface treatment or the like of the workpiece W, and has various component compositions depending on the nature of the workpiece W treatment. The vapor deposition material Gz is stored in the storage container 4 in the form of powder, granules, pellets or sheets.

  The mounting table 7 is a table on which the storage container 4 is mounted. The mounting table 7 is installed such that the storage container 4 is mounted at a position where the electron beam of the electron gun 5 reaches. The mounting table 7 may be configured such that a plurality of storage containers 4 are mounted and each storage container 4 is moved to an irradiation position where the electron beam reaches. When a plurality of storage containers 4 are mounted and moved, the mounting table 7 is configured to move in accordance with a preset program procedure or to be moved by an external operation.

  As shown in FIGS. 1 and 2, the sublimation pump 10 is a pump used to evacuate the inside of the housing 2. The sublimation pump 10 is a pump that is used alone or together with other vacuum pumps to form a vacuum in the vacuum processing chamber 2a. The sublimation pump 10 is attached to the side wall of the housing 2 here. The sublimation pump 10 is installed in the vacuum processing chamber 2a, installed in a spare chamber adjacent to the vacuum processing chamber 2a, or connected to the vacuum processing chamber 2a via a pipe or the like. Used in the embodiment.

  As shown in FIG. 2, the sublimation pump 10 includes a filament 12 formed of a Si-based material, a support 13 that supports an end of the filament 12, and a melting point of the filament 12 supported on the support 13. A power source (gas phase means) 15 for heating and sublimating below, and a deposition plate (cylindrical body) disposed facing the filament 12 to deposit the Si-based material sublimated from the filament 12 via the power source 15 ) 16, a shield plate 17 in which an air inlet 17 a for sucking the gas in the vacuum processing chamber 2 a is formed, and a cooling means 19 provided outside the deposition plate 16. This sublimation pump 10 forms a Si-based material deposited film 18 by sublimating and depositing a Si-based material filament 12 on a deposition plate 16, and a Si dangling bond of the formed Si-based material deposited film 18. Thus, the vacuum state in the vacuum processing chamber 2a is quickly realized.

  The filament 12 is formed of a Si-based material, and is sublimated by being heated to a melting point or lower by energization from the power source 15. The filament 12 is formed in the filament by a material of any one of Si, Si alloy, Si compound, and Si mixture (including Si oxide, Si nitride, Si oxide + α, and Si nitride + α). . And the filament 12 is supported by the support body 13 in the state which twisted the filament. The filament 12 is particularly preferably used as a Si alloy. That is, when the filament 12 is processed into a striate body, Si becomes an alloy or a mixture with a metal, thereby facilitating processing such as extending or thinning. Examples of the Si alloy or Si mixture include Si (silicon) and the following metals. That is, as an alloy or a mixture, Ti (titanium), Zr (zirconium), Nb (niobium), Ta (tantalum), Cr (chromium), Mo (molybdenum), W (tungsten), Mn (manganese), Fe (iron) ), Co (cobalt), Ni (nickel), and Mg (magnesium), and the ratio is in the range of (10 mol% ≦ Si ≦ 90 mol%).

Or Si (silicon);
Al (aluminum), Cu (copper), Zn (zinc), Ru (ruthenium), Rh (rhodium), Pd (palladium), Ag (silver), Sn (tin), Sb (antimony), Te (tellurium), It is a mixture (10 mol% ≦ Si ≦ 90 mol%) composed of at least one of Re (rhenium), Ir (iridium), Pt (platinum), Au (gold), C (carbon), and Ge (germanium).

  The support 13 supports the filament 12 and can conduct electricity from the power source 15 to the filament 12. The support 13 may be an existing one as long as it is a configuration used in a sublimation pump. Here, the support 13 is installed on the support plate 14 to support one end of the filament 12, and a fixing plate 13b that supports the other end of the filament 12 fixed to the mounting fixing portion 13a. A support column 13c that supports the fixed plate 13b on the support plate 14 is provided. The support 13 is not particularly limited as long as it can fix the filament 12 and perform the sublimation work of the filament 12.

The power source 15 is for heating the filament 12 supported by the support 13. The power source 15 may be an existing power source that can supply power that can be heated to a temperature at which the filament 12 is sublimated (melting point or lower).
The deposition plate 16 is a cylindrical body installed around the filament 12 supported by the support 13, and is for forming a deposition film 18 by sublimation of the filament 12. Here, the deposition plate 16 is installed on the side wall of the casing 2 (vacuum processing chamber 2a). The deposition plate 16 is not particularly limited as long as it is used for the existing sublimation pump 10.

The shield plate 17 communicates with the vacuum processing chamber 2a to form an intake port 17a for sucking gas from the vacuum processing chamber 2a. The suction port 17a and the cooling means 19 allow the sublimate from the filament 12 to be vacuum processed. It is possible to prevent scattering to the chamber 2a. If this shield board 17 is used for the existing sublimation pump 10, it will not be specifically limited.
The cooling means 19 suppresses the influence of heat generated when the filament 12 is heated, and the vapor-phase Si-based material formed by sublimation of the filament 12 is cooled without flowing into the vacuum processing chamber. It is for adsorbing on the inner surface of the deposition plate 16 to form a deposited film of Si-based material. Here, the cooling means 19 is configured to cool the deposition plate 16 by providing a pipe through which a coolant such as water or liquid nitrogen flows on the outer wall of the deposition plate 16. The cooling liquid supply means (not shown) of the cooling means 19 is installed outside the housing 2.

Next, a vacuum suction method in the vacuum processing chamber will be described with reference to FIG. 3 mainly with reference to FIGS. Note that the case where a Si-based material is used for the filament of the sublimation pump 10 will be described. Here, the case where the inside of the vacuum processing chamber 2a is evacuated and the surface of the workpiece W is subjected to vapor deposition processing will be described.
First, the workpiece W is held by the holding mechanism 3 in a state where the opening / closing lid 2b of the housing 2 is opened, and is installed at a position facing the storage container 4 of the vacuum processing chamber 2a. The sublimation pump 10 including the Si-based material filament 12 is installed so as to communicate with the vacuum processing chamber 2a (step S1).
In the vacuum processing apparatus 1, when the workpiece W is installed, the inside of the housing 2 is evacuated by the main vacuum pump Ps (step S2).

  In the vacuum processing apparatus 1, when the sublimation pump 10 that performs vacuum suction is operated, the filament 12 formed of the Si-based material of the sublimation pump 10 is heated by the power supply 15 and sublimated to generate a gas-phase Si-based material. Vacuum suction is performed while forming the material as the Si-based material deposition film 18 (S3). Therefore, in the vacuum processing apparatus 1, the sublimation pump 10 is operated to form the Si-based material deposited film 18, so that the vacuum existing in the housing 2 is unnecessary due to the adsorption action of Si dangling bonds. The component molecules are removed by being adsorbed on the deposited film 18.

In the vacuum processing apparatus 1, thereafter, the vapor deposition material Gz in the storage container 4 is heated by the electron beam from the electron gun 5 and evaporated by the electron gun 5, and the vapor deposition material Gz is formed on the surface of the workpiece by opening the shutter mechanism 6. Is vapor-deposited (step S4). Note that the workpiece W is subjected to vapor deposition while performing vacuum suction (step S4).
Next, when the first vapor deposition process is completed, it is determined whether or not the process of the setting conditions set in advance for the workpiece W is completed (step S5), and the process ends when the process is completed (step S5). S5 Yes). If it is determined that the process has not ended (No in step S5), the next process is performed.

  When the next process is performed, the vacuum suction operation is performed again according to the set conditions, and the vacuum may be adjusted to the initially set degree of vacuum. When vacuum processing is performed again, vacuum suction is performed only by the main vacuum pump Ps without operating the sublimation pump 10 while maintaining the current vacuum state in the housing 2 (without venting). And when vacuum suction is performed again by both the main vacuum pump Ps and the sublimation pump 10. Then, by operating the sublimation pump 10, a deposited film 18 of Si-based material is formed, and component molecules unnecessary for the vacuum existing in the housing 2 are removed by the adsorption action of Si dangling bonds. . Then, when the vacuum state reaches the set condition, the workpiece process and vacuum suction (step S4) for performing the process on the surface of the workpiece W are performed again, and it is determined whether or not the setting process is finished, and the setting process is performed. Steps S4 and S5 are repeated until is finished.

  In the vacuum suction method described above, when a sublimation pump is used, as shown in FIGS. 4 (a) and 4 (b), an adsorption action on the deposited film 18 of the Si-based material occurs. In other words, in the deposited film 18, not all the bonding states of Si are established on the crystal surface and inside the crystal, and bonding defects generally occur. Accordingly, the sublimation pump 10 causes an action of adsorbing Si dangling bonds in the deposited film 18 of the Si-based material due to the operation thereof, and adsorbs the component molecules unnecessary for the vacuum to the defective portion where there is no bonding partner. It can proceed to a vacuum state. In the deposited film 18, since Si atoms on the surface of the Si-based material deposited film 18 do not have a partner to be bonded outside the crystal, Si dangling bonds are easily formed on the surface of the deposited film 18.

  Further, the deposited film 18 has Si dangling bonds at the defects if there is a defect that does not have a bonding partner inside even if the Si-based material is a single crystal. You can bond. In the covalently-bonded Si crystal, two atoms to be bonded emit electrons one by one, and the two electrons occupy the bond orbit of the atom pair to form a strong and stable bonded state. Therefore, the bond that has lost its bond partner, that is, the Si dangling bond, is rich in reactivity, that is, has high chemical activity, and causes recombination and trapping. That is, in the deposited film 18, the high chemical activity of the Si dangling bonds becomes a driving force (Motive Force) of the adsorption effect of the Si-based material, and atoms unnecessary for vacuum can be removed.

  Further, in the vacuum suction method, even when the sublimation pump 10 is used simultaneously with the main vacuum pump Ps, since the Si-based deposited film is formed, it is unnecessary to be quickly evacuated due to the adsorption action of Si dangling bonds. Component molecules are removed. By forming the Si-based deposited film, the vacuum processing can be performed quickly as with Ti. When the degree of vacuum reaches the set condition, the surface treatment work of the workpiece W is performed by the same procedure as described above.

Next, a sputtering apparatus and a vacuum suction method as the vacuum processing apparatus 100 according to the present invention will be described with reference to FIG.
The vacuum processing apparatus 100 includes a casing 102, a holding unit 103 that holds the workpiece W in the casing 102, a mounting table 104 for the target Tg, and an operating unit (gas phase unit) that applies a voltage to the workpiece W and the target Tg. 105 and a preliminary chamber 101 for depositing a Si-based material. In addition, the vacuum processing apparatus 100 performs the processing operation in the casing 2 in a state where a predetermined gas atmosphere is provided by the atmospheric gas supplied from the atmospheric gas container Fg connected to the inside through the introduction portion 2d. Done.

  The preliminary chamber 101 includes an indoor deposition wall surface 101a for forming the Si-based deposition film 101d, an Si-based target 101c for forming the Si-based deposition film 101d on the indoor deposition wall surface 101a, and sputtering the Si-based target 101c. Thus, the second operating means (vapor phase means) 101e for forming the Si-based deposition film 101d is provided.

  The indoor deposition wall surface 101 a is a housing that is installed in the housing 102 and has a communication port 101 h that communicates with the housing 102. Here, the indoor deposition wall surface 101 a is formed of the same material as the inner wall of the housing 102. The indoor deposition wall surface 101a is for forming a Si-based deposition film 101d on at least a part of the wall surface. The indoor deposition wall surface 101a is installed in a position where there is no influence of the processing of the workpiece W in the housing 102. In FIG. 5, the preliminary chamber 101 is disposed on the side opposite to the suction path of the main vacuum pump Ps. However, the spare chamber 101 may be disposed between the workpiece W and the main vacuum pump Ps.

The indoor deposition wall surface 101a is formed with a communication port 101h, which is an intake port that communicates with the vacuum processing chamber 102a and sucks gas from the vacuum processing chamber 102a. The Si-based target is formed by the communication port 101h and the cooling means 101b. It is possible to prevent the vapor phase of the Si-based material generated from 101c from scattering into the vacuum processing chamber 102a.
The cooling unit 101b suppresses the influence of heat generated by plasma discharge or sputtering of the Si-based target 101c, and causes the Si-based material in a vapor phase generated by the sputtering of the Si-based target 101c to the vacuum processing chamber 102a. This is for forming the Si-based deposited film 101d of the Si-based material by adsorbing to the inside of the cooled indoor deposition wall surface 101a without being swelled. The cooling means 101b is configured to cool the indoor deposition wall surface 101a by providing a pipe through which a coolant such as water or liquid nitrogen flows on the outer wall of the indoor deposition wall surface 101a.

  The Si-based target 101c is made of any material of Si, Si alloy, Si compound, and Si mixture, and is made of the same material as the Si-based material already described in the sublimation pump 10, so that it can be used as a sputtering target. Is formed. This Si-based target 101c is used to form a Si-based deposition film 101d in the indoor deposition wall surface 101a by sputtering by applying a voltage to the indoor deposition wall surface 101a by the second actuating means 101e.

  The second operating means 101e is for applying a voltage to the Si-based target 101c and the indoor deposition wall surface 101a that are electrically connected to cause the Si-based target 101c to be sputtered. This 2nd action | operation means 101e is equipped with the structure equivalent to what is used with a general sputtering device.

  The housing 102 includes a vacuum processing chamber 102a, an opening / closing lid 102b, and a connection portion 102c for the main vacuum pump Ps. The casing 102 is not limited as long as it can be used as a sputtering apparatus.

  The holding means 103 holds the workpiece W at a position where it can be sputtered. The holding means 103 has a general configuration so that it can be electrically connected to the workpiece W so that it can be sputtered.

  The mounting table 104 is for mounting the target Tg. The mounting table 104 is configured such that a voltage can be applied between the workpiece W and the target Tg while being electrically connected to the holding means 103 that holds the target Tg. The mounting table 104 mounts a plurality of targets Tg, switches the electrical connection between each target Tg and the operating means 105 (gas phase means), and electrically connects each target Tg and the workpiece W. You may comprise so that it can connect.

  The operating means 105 is for sputtering from the target Tg toward the workpiece W. The actuating means 105 is for electrically connecting, for example, applying a voltage between the workpiece W and the target Tg, and sputtering the target Tg to treat the surface of the workpiece W. The actuating means 105 has a configuration capable of applying a voltage by electrically connecting the target Tg and the workpiece W, for example, in the case of a direct current sputtering method, a high frequency sputtering method, or a high frequency magnetron sputtering method. The actuating means 105 may be configured to sputter the target Tg using an ion gun.

The case of operating the vacuum processing apparatus 100 will be described with reference mainly to FIG. 6 (also refer to FIG. 5).
First, in the vacuum processing apparatus 100, the opening / closing lid 102b of the casing 102 is opened to hold the workpiece W on the holding means 103, and the Si target 101c is installed in the spare chamber 101 (step S11). The lid 102b is closed.
Then, vacuum suction is performed by the main vacuum pump Ps to evacuate the inside of the housing 2 and the preliminary chamber 101 (step S12), and then the Si-based target 101c in the preliminary chamber 101 is sputtered to form the Si-based material on the indoor deposition wall surface 101a. A deposited film 101d is formed (step 13).

  In this vacuum processing apparatus 100, the second operating means 101e of the preliminary chamber 101 is operated to sputter the Si-based target 101c to form the Si-based deposited film 101d on at least a part of the indoor deposition wall surface 101a. The timing for forming the Si-based deposited film 101d is during operation of the main vacuum pump Ps. Since the Si-based deposited film 101d is formed when the main vacuum pump Ps is operated, the Si dangling bond is adsorbed, and component molecules unnecessary for vacuum are bonded to the Si-based deposited film 101d. Vacuum suction can be advanced more quickly by adsorbing to a defective part where there is no counterpart.

  In the vacuum processing apparatus 100, when the vacuum state reaches a preset condition (step 14), the second operating means 101e of the preliminary chamber 101 is stopped when it is simultaneously operating, and sputtering from the Si-based target 101c is performed. Processing is also stopped. Then, in the vacuum processing apparatus 100, the surface treatment work of the workpiece W is performed by sputtering from the target Tg toward the workpiece W via the operating means 105 (step 15). When the surface of the workpiece W is processed by sputtering, the atmospheric gas is introduced from the atmospheric gas container Fg through the introduction part 2d.

After the first processing is performed on the surface of the workpiece W, the vacuum processing apparatus 100 determines whether or not the processing of the setting conditions set in advance for the workpiece W is completed (step S16). If completed, the process ends (Yes in step S16). If it is determined that the process has not ended (No in step S16), the processes in steps S14 and S15 are performed again.
Note that in the vacuum processing apparatus 100, before the processing is performed again, the vacuum state is measured again, and if the vacuum condition is not satisfied, the first vacuum state is performed. At this time, if the Si-based deposition film 101d is already formed on the indoor deposition wall surface 101a of the preliminary chamber 101 and the Si dangling bond remains, the adsorbing action of the Si dangling bond continues and is unnecessary for the vacuum. It is possible to remove various component molecules.

Further, the main vacuum pump Ps may be operated while the Si-based target 101c in the preliminary chamber 101 is sputtered by the second operating means 102d to form the Si-based deposited film 101d on the indoor deposition wall surface 101a of the preliminary chamber 101. . In this way, even if most of the defects (Si dangling bonds) in the Si-based deposited film are filled with the adsorbed gas, a large amount of defects (Si dangling bonds) are formed on the indoor deposition wall surface of the preliminary chamber 101. A new Si-based deposited film is formed, and the vacuum processing chamber 102a can be quickly evacuated to a vacuum state under a set condition by using the adsorption force.
In the vacuum processing apparatus 100, when vacuuming the inside of the housing 102 by the main vacuum pump Ps, one of the plurality of targets Tg is made of Si-based material, and this Tg is used to store the inside of the vacuum processing chamber 102a. A Si-based deposited film may be formed on the surface of the workpiece W to activate the Si dangling bond adsorption action. In the vacuum processing apparatus 100, a Si-based deposited film can be prevented from being formed on the surface of the workpiece W by a shutter (shutter mechanism) 6 installed in the immediate vicinity of the workpiece W (see FIG. 5).

  As a result, in the vacuum processing apparatus 100, when the same vacuum state is obtained as compared with the state in which the conventional vacuum suction is performed, it can be achieved in 1/2 time (see Table 3). Further, in the vacuum processing apparatus 100, in the same vacuum suction time, for example, a vacuum state after 1 minute and 30 seconds, it can be improved as a difference in the degree of vacuum (Pa) which is different by one digit at maximum (see Table 2).

  In the vacuum processing apparatus 100, the opening / closing lid 102 b of the housing 102 is opened, a new workpiece W is placed on the holding means 103, and the surface treatment of the workpiece W is performed by ensuring the vacuum state by repeating the above-described steps again. be able to. When the mounting table 104 mounts a plurality of targets Tg, the target Tg connected to the operating means 105 is switched, and the work on the workpiece W is continued with the next target Tg without releasing the vacuum state. be able to.

Next, the vacuum processing apparatus 200 will be described with reference to FIG.
As shown in FIG. 6, the vacuum processing apparatus 200 includes a Si-based deposited film forming unit 201 that forms a Si-based deposited film 201 d installed in a preliminary area installed in the housing 202, and a work W on the housing 202. Holding mechanism 203 for holding and installing, shutter mechanism 206 for controlling the surface treatment of workpiece W held by holding mechanism 203, and crucible for storing target Tg or vapor deposition material Gz for performing the surface treatment of workpiece W The mounting table 204 for mounting the storage container 204a, etc., and the operating means 205 for applying a voltage between the target Tg of the mounting table 204 and the work W of the holding mechanism 203, or the vapor deposition material in the storage container 204a is melted. And an operating means (not shown) for energizing and heating the electron gun or the storage container 204a.

  The Si-based deposited film forming unit 201 includes a deposition plate 201a for depositing the Si-based deposited film 201d, a storage container 201b for storing a Si-based material 201c installed at a position facing the deposition plate 201a, and the storage container 201b. Second operating means 201e for placing and heating the container 201b.

  The deposition plate 201a is installed at a position that does not affect the surface treatment work of the workpiece W. Here, the one end side is bent at a predetermined angle so that the Si-based material to be deposited does not scatter to the workpiece W side. . In this deposition plate 201a, the surface side on which the Si-based deposition film 201d is formed is formed of the same material as the inner wall of the housing 2 here. In this deposition plate 201a, it is not necessary to receive all of the deposited Si-based deposited film 201d. If the shutter mechanism 206 is closed, the deposited plate 201a is shielded from the deposited Si-based material so as not to affect the surface treatment of the workpiece W. Therefore, the Si-based deposition film 201d may be formed on a part of the inner wall surface of the housing 202 (vacuum processing chamber 202a). Note that when the Si-based deposition film 201d is formed on the inner wall surface of the vacuum processing chamber 202a, the area of the Si-based deposition film is increased and the adsorption force of Si dangling bonds is increased. Is advantageous.

  The storage container 201b stores a Si-based material, and is a crucible or boat that can heat and melt the Si-based material. The shape of the Si-based material stored in the storage container 201b is any of powder, granules, sheets, pellets, or a combination thereof. This Si-based material is made of any material of Si, Si alloy, Si compound, and Si mixture (including Si oxide, Si nitride, Si oxide + α, and Si nitride + α). The Si-based material is, for example, Si (silicon) and the following metals as the Si alloy or Si mixture. That is, as an alloy or a mixture, Ti (titanium), Zr (zirconium), Nb (niobium), Ta (tantalum), Cr (chromium), Mo (molybdenum), W (tungsten), Mn (manganese), Fe (iron) ), Co (cobalt), Ni (nickel), and Mg (magnesium), and the ratio is in the range of (10 mol% ≦ Si ≦ 90 mol%).

Alternatively, as an alloy or mixture, Si (silicon),
Al (aluminum), Cu (copper), Zn (zinc), Ru (ruthenium), Rh (rhodium), Pd (palladium), Ag (silver), Sn (tin), Sb (antimony), Te (tellurium), It is a mixture (10 mol% ≦ Si ≦ 90 mol%) composed of at least one of Re (rhenium), Ir (iridium), Pt (platinum), Au (gold), C (carbon), and Ge (germanium).

  The second actuating means (means for bringing the Si-based material into a vapor phase) 201e heats the Si-based material in the storage container 201b so as to be melted and deposited. The second actuating means 201e is not limited as long as it can heat the Si-based material in the storage container 201b to vapor-deposit the Si-based material on the deposition plate 201a.

The housing 202 is capable of performing a process such as vapor deposition by making the inside vacuum, and penetrates the vacuum processing chamber 202a, an open / close lid 202b provided on the upper portion of the vacuum processing chamber 202a, and the outer wall of the vacuum processing chamber 202a. And a connecting portion 202c connected to the main vacuum pump Ps.
The holding mechanism 203 holds the workpiece W processed in the housing 202. The holding mechanism 203 only needs to have a configuration capable of holding the workpiece surface to be processed so as to expose the workpiece W, and can further rotate the workpiece surface in a direction parallel to the horizontal plane. The configuration is not limited as long as it has a configuration capable of cooling or heating the surface.

  The mounting table 204 is used to install either the target Tg or a storage container (such as a crucible or a boat) 204a, and both are collectively shown in the drawing. The mounting table 204 may have a configuration in which a plurality of targets Tg or a plurality of crucibles or boats are mounted, and a shutter that can be independently opened and closed is disposed immediately above each target Tg or crucible boat. When a plurality of targets Tg or storage containers 204a are mounted, the mounting table 204 is electrically connected to the actuating means 205 in accordance with a preset program procedure or by remote operation from the outside. It is configured to be switched.

The operating means 205 is a means for applying a voltage to the workpiece W when the target Tg is on the mounting table 204, and the second operating means 201e when the storage container 204a is on the mounting table 204. It is a means to heat to become the same structure.
The shutter mechanism 206 is formed by sputtering from the target Tg or evaporation from the vapor deposition material Gz stored in the storage container 204a, and the Si-based material stored in the storage container 201b that the deposition plate 201a cannot receive (cannot be shielded). It controls the deposition from the material. In the shutter mechanism 206 for achieving these objects, the shutter is installed between the target Tg or the storage container 204a and the processing path facing the workpiece W, and the shutter is provided in all or part of the processing path. The deposition operation or the sputtering operation is controlled such that the deposition operation or the sputtering operation is performed by blocking the position by moving or by blocking the shutter from moving to the retracted position from the processing path. The shutter mechanism 206 is not particularly limited as long as it has a structure capable of blocking and blocking the vapor deposition operation or the sputtering operation.

  The target Tg or the vapor deposition material Gz is a material used for the surface treatment of the workpiece W, and various component compositions are used depending on the component of the workpiece W and the nature of the treatment, and a plurality of targets Tg or a plurality of vapor deposition materials. At least one of Gz is made of Si-based material, and the deposition mechanism or sputtering operation on the workpiece W is shut off by the shutter mechanism 206, and then the Si-based deposited film exhibiting an adsorption action due to Si dangling bonds is vacuumed. You may form in the process chamber 202a inner wall and the shutter mechanism 206 lower surface. The target Tg is formed in a bulk shape, and the vapor deposition material Gz is stored in the storage container 204a in the form of powder, granules, pellets or sheets, or a combination thereof.

When the vacuum processing apparatus 200 is operated, the operation is as follows.
First, in the vacuum processing apparatus 200, the opening / closing lid 202b of the housing 202 is opened, the work W is held by the holding mechanism 203, the opening / closing lid 202b is closed, and the inside of the housing 202 is vacuumed by the main vacuum pump Ps. .
In the vacuum processing apparatus 200, when the main vacuum pump Ps is operated, the second operating means 201e of the Si-based deposited film forming unit 201 is operated, and the Si-based material 201c is heated and evaporated to form the Si-based deposited film 201d. Formed on the deposition plate 201a. In this way, by forming the Si-based deposition film 201d on the deposition plate 201a or a part of the vacuum processing chamber 202a while operating the main vacuum pump Ps, dangling bonds are adsorbed and are unnecessary for vacuum. Thus, vacuum suction can be advanced more quickly by adsorbing the component molecules to the defective portion of the Si-based deposited film 201d that does not have a Si atom bonding partner.

  In the vacuum processing apparatus 200, when the vacuum state reaches a preset condition, that is, the degree of vacuum (attainment degree of vacuum), the second operating unit 201e of the Si-based deposited film forming unit 201 is stopped to stop the Si-based material 201c. The deposition process is temporarily stopped. Even if the surface treatment method of the workpiece W is either vapor deposition or sputtering, the main vacuum pump Ps does not stop because the gas generated by the surface treatment is quickly exhausted after the surface treatment is finished. In the vacuum processing apparatus 200, the surface treatment of the workpiece W is performed by sputtering or vapor deposition from the target Tg or the vapor deposition material Gz toward the workpiece W via the operating unit 205.

In the case of sputtering, the main valve is adjusted (mostly closed), and the gas pressure (sputtering gas pressure) in the vacuum processing chamber 202a is kept at the set condition by the balance between the amount of gas introduced for sputtering and the amount of exhaust gas. Surface treatment of the workpiece W is performed. The ultimate vacuum is in the range of 10 ⁻⁵ to 10 ⁻⁶ Pa, whereas the gas pressure during the surface treatment by sputtering is in the range of 10 to 10 ⁻¹ Pa. In the case of vapor deposition, the main valve is fully opened, and the surface treatment of the workpiece W is performed while the gas generated by heating the crucible or boat is exhausted by the main vacuum pump Ps. In the case of vapor deposition, it is desirable that the degree of vacuum in the vacuum processing chamber 202a during the surface treatment is not deteriorated as much as possible from the degree of vacuum before the surface treatment, that is, the ultimate degree of vacuum. For this reason, the main valve is fully opened.

  The vacuum processing apparatus 200 performs the following process on the surface of the workpiece W when the surface treatment of the workpiece W is repeated so that the materials of the adjacent layers are different in order to produce a multilayer film such as an optical disk. Previously, the vacuum state is measured again, and if the vacuum condition is not satisfied, an operation to make the vacuum state before starting the first surface treatment is performed. At this time, since the Si-based deposition film 201d is already formed on the inner wall surface or the deposition plate 201a in the housing 202, defects that are not filled with the adsorbed gas, that is, Si dangling bonds remain in this. For example, the adsorbing action of the Si dangling bonds can be continued and unnecessary component molecules can be removed. In the vacuum processing apparatus 200, the operation of heating and depositing the Si-based material 201c of the Si-based deposited film forming unit 201 by the second operating means 201e during the vacuuming operation before starting the first surface treatment. The main vacuum pump Ps may be operated while performing again. This is filled with the adsorbed gas remaining on the inner wall surface in the housing 202 or the Si-based deposition film 201d formed on the deposition plate 201a during the vacuuming operation before starting the first surface treatment. This is a method for compensating for a case where there are few Si dangling bonds that are not present and sufficient adsorption of Si dangling bonds cannot be expected.

  As a result, in the vacuum processing apparatus 200, the same vacuum state can be achieved in half the time compared to the state in which the conventional vacuum suction is performed (see Table 3). Further, in the vacuum processing apparatus 200, in the same vacuum suction time, for example, in a vacuum state after 1 minute and 30 seconds, it can be improved as a difference in the degree of vacuum (Pa) which is different by one digit at maximum (see Table 2).

Next, examples of the present invention will be described. In addition, this invention is not limited to this Example.
In the embodiment according to the present invention, the medium configuration of an optical disk for a recording experiment of high-speed and large-capacity optical recording and an optical disk for a gap servo experiment were performed. In addition, experiments were conducted using a 6-element magnetron sputtering apparatus. This 6-element magnetron sputtering system has the following main components: vacuum chamber, cryopump (CP, main pump), dry pump (DRP, roughing pump), 6-element cathode (6-element target)), two high-frequency power supplies Control rack (with LCD touch panel).
In an optical disk for recording experiments, a multilayer film having the following layer structure was deposited on a substrate (PC (Polycarbonate) Subst.).
_{Si-N / ZnS-SiO 2} / Ge-Bi-B-O / ZnS-SiO 2 / Si-N / Ag-a.

Further, in the optical disk of the gap servo experiment, a two-layer film having the following layer structure was deposited on a substrate (PC Subst).
Si-N / Ag-a.
Ag-a is an Ag alloy containing Bi. Ge-Bi-B-O is a so-called write once recording material that cannot be erased and cannot be rewritten once it has been written by irradiating a laser beam focused by an objective lens. .

  Table 1 shows the film forming conditions other than the sputtering time when the optical disk medium described above is produced by the magnetron sputtering method.

Based on the above structure, the target (material) is switched to produce a multilayer optical disk. Ultimate vacuum before starting the discharge for forming a film of the first layer is a 6 × ¹⁰ -5 Pa~3 × about ¹⁰ -5 Pa. The layers other than Si—N (silicon nitride) were prepared with targets whose compositions were adjusted, but the Si—N (silicon nitride) layer was formed from a Si target doped with B and Ar (argon) · N ₂ ( Nitrogen) was used to form a film by a reactive sputtering method using a mixed gas, but a Si—N target may be used.
During discharge, a vacuum chamber, a cathode mounted with a target backed by a copper backing plate, and a PC (Polycarbonate) substrate are mounted to prevent mass emission of impurity gases and damage to the target. Cool by passing water through the turntable.

In addition, in order to suppress the entry of impurities such as oxygen into each layer as much as possible, the degree of vacuum is 6 × 10 ⁻⁵ before the first discharge before starting the discharge for forming the next layer. Long evacuation is performed so as to be close to about Pa to 3 × 10 ⁻⁵ Pa. In the process of producing the above medium, the pumping speed after forming an Si—N (silicon nitride) layer and stopping the introduction of Ar (argon) / N ₂ (nitrogen) gas for discharge and sputtering is as follows: These three materials, namely, Ag alloy, ZnS—SiO ₂ , and Ge—Bi—B—O are faster than the exhaust speed after film formation. This is because, although the film deposited on the adsorption surface such as the vacuum chamber wall is Si—N, not all the Si atoms on the film surface are terminated with N, and a lot of Si dangling is formed on the film surface. It shows that there is a ring bond, and there is a Si dangling bond inside the film due to defects and grain boundaries, and the adsorption action is working.
In addition, from this, even when Si—O, an alloy containing Si, or a mixture is formed instead of the Si film, if the Si dangling bond is formed on the film surface, it is considered that the adsorption action works. .

The adsorption action of Si dangling bonds, which is a method according to the present invention, will be described.
The sublimation pump 10 used the components of the filament 12 as follows.
Si or an alloy or mixture of Si and at least one of Ti, Zr, Nb, Ta, Cr, Mo, W, Mn, Fe, Co, Ni, Mg (10 mol% ≦ Si ≦ 90 mol%) Or a mixture of Si and at least one of Al, Cu, Zn, Ru, Rh, Pd, Ag, Sn, Sb, Te, Re, Ir, Pt, Au, C, Ge (10 mol% ≦ The filament 12 is made of (Si material) with Si ≦ 90 mol%.

  The filament 12 made of Si-based material is energized from the power source 15, and the filament 12 is heated and sublimated to 1412 ° C. or lower, which is the melting point of Si, or lower than the melting point of the Si-based material. Since the Si-based deposited film is present in the housing 2 (see FIG. 1), it is possible to evacuate to a vacuum state due to the adsorption action of the Si dangling bonds formed on the adsorption surface by the Si-based deposited film.

  Example of vacuum evacuation operation using Si dangling bond adsorption action after forming Si-N film using magnetron sputtering apparatus and adding Si-N film and stopping discharge (Example 1) Indicates.

Table 2 shows the comparison of the exhaust speed after the end of each layer discharge when the Si-N / Ag-a bilayer film (Si-N (15 nm) / Ag-a (50 nm) / PCsubst.) Is produced.
The Ag-a film deposition conditions were Ar flow rate = 60 sccm, sputtering gas pressure = 0.7 Pa, sputtering power = 70 W, sputtering time = 6 minutes 23 seconds.
The Si—N film deposition conditions were Ar / N ₂ flow rate ratio = 60/10, sputtering gas pressure 0.7 Pa, sputtering power = 70 W, sputtering time = 12 minutes 15 seconds.

Despite the formation of the Si-N film, there are a large number of Si dangling bonds on the adsorption surface. Therefore, the exhaust speed after stopping the discharge for forming the Si-N film is Ag. -A The exhaust speed is higher than after the discharge for film formation is stopped, and reaches 5.46 × 10 ⁻⁵ Pa at 1 minute 30 seconds after the discharge is stopped. On the other hand, in the case of the Ag-a film formation in which the adsorption action is hardly seen, the degree of vacuum at the time of 1 minute 30 seconds after the discharge is stopped is only 1.45 × 10 ⁻⁴ Pa.

Example 1 shows the improvement effect of the exhaust speed when Si dangling bonds exist on the adsorption surface by comparing the ultimate vacuum in a relatively short time (after 1 minute 30 seconds) after stopping the discharge. Yes.
Next, as Example 2, a Bi—B—O single layer film or a Si—N single layer film was formed on a glass substrate with the same magnetron sputtering apparatus as in Example 1, and was evacuated for a long time without breaking the vacuum. The difference in ultimate vacuum is shown. The film forming conditions for the Bi—B—O film are Ar flow rate = 60 sccm, sputtering gas pressure = 0.35 Pa, sputtering power = 70 W, and film forming time = 5 minutes.
The deposition conditions of the Si—N film are Ar / N ₂ flow rate ratio = 60/5, sputtering gas pressure = 0.7 Pa, sputtering power = 70 W, sputtering time = 1 hour 7 minutes 45 seconds.
Table 3 shows the comparison of ultimate vacuum.

When a Si-N film having an adsorption action by Si dangling bonds is formed, the ultimate vacuum when evacuating for 22 hours, 20 minutes and 15 seconds without venting after the discharge is stopped is 3.55 × 10 ⁻⁵ Pa. The Bi—B—O film having no adsorption effect was formed, and the vacuum was higher than the ultimate vacuum when the discharge was stopped for 45 hours and 2 minutes more than doubled. Therefore, the adsorption effect of Si dangling bonds formed in the Si-N film on the adsorption surface is maintained even without evacuating for a long time (without the adsorbed gas separating), leading to improvement in the ultimate vacuum. I understand that.
In Examples 1 and 2, the Si-N film was formed only once (preparation of the adsorption surface), but in the film formed by adsorbing exhausted gas and forming Si dangling bonds. If it disappears, the adsorption surface does not perform the exhaust operation. Therefore, in the vacuum processing apparatus, the clean adsorption surface having the adsorption action of the Si dangling bonds may be regenerated by repeating the deposition of the Si—N film with the exhaust by another type of pump interposed therebetween.

<Explanation of Experiments in Examples>
The gas pressure during sputtering film formation is 0.7 Pa. This pressure depends on the balance between the amount of gas introduced and the amount of gas exhausted so that the gas pressure generated by adding the gas generated by plasma discharge or sputtering of the target to the gas introduced from the outside into the vacuum chamber is constant. The pressure is determined. Therefore, the higher the sputtering power and the longer the sputtering time, the more gas is generated in the vacuum chamber, but the vacuum chamber gas pressure (degree of vacuum) at the end of sputtering is always 0 regardless of the sputtering power and sputtering time. .7 Pa (This pressure value is a set value and can be changed. In the embodiment, 0.7 Pa). In order to compare the evacuation capacity of the film formed using each target, it is considered that the evacuation capacity of the main pump CP is always constant, the gas introduction valve is closed, and the MV is fully opened for 1 minute. The degree of vacuum after 30 seconds was confirmed and compared.

<Concept of Si component composition (composition ratio)>
If even a small amount of Si is mixed in the target, it is considered that there is an evacuation effect due to Si dangling bonds in the Si-based thin film. The specific% (mol%) of Si is as follows.
The composition ratio (molar ratio (mol%)) between ZnS and SiO ₂ of the ZnS—SiO ₂ target used in the examples of the present invention is 80:20. The composition ratio (mol%) of Si in SiO ₂ is 1/3, that is, 33%. Therefore, the composition ratio (mol%) of Si in the entire ZnS—SiO ₂ is 6.6% (= 33 × 0.2).
When a film is formed from a ZnS—SiO ₂ target, the evacuation effect is clearly confirmed. Therefore, it is considered that the target should contain 5% or more of Si. It can be seen that the vacuum exhaust performance of the Si-based thin film increases as the proportion of Si in the alloy or compound increases.

As described above, in the embodiment or the example according to the present invention, the vacuum state is formed by forming the Si-based material deposited film and performing vacuum suction so that the Si-based material deposited film is adsorbed by the dangling bonds. It becomes possible to form quickly. Although the present invention has been described as a deposited film of a Si-based material, it may be monocrystalline, polycrystalline, or amorphous, or may have a structure in which a deposited layer is stacked, and adsorbs Si dangling bonds. As long as the action is generated, the crystal, the amorphous state, the formation position (surface, inside the crystal), the film thickness, the layer thickness, the width, and the form are not limited.
In each of the above-described embodiments, the vacuum state may be formed by a combination as shown below.
That is, the location of the Si-based material and the vapor phase means, the vapor phase method, the formation timing of the Si-based deposited film, what was used as the vacuum suction action, and the combination with the atmosphere may be as follows. Absent.

  The installation location of the Si-based material and the heating means (A: vacuum processing chamber, B: preliminary chamber) was used, and the heating method (2: sputtering, 3: sublimation, 4: evaporation) was used. Further, depending on the combination of these factors, what is used as the vacuum suction action at the timing of formation of the Si-based deposited film (A: during formation, yes: after formation) (a: film suction action, vacuum treatment) The following cases may be used when the vacuum is applied to the chamber (b: a vacuum pump provided in the vacuum processing apparatus) and the atmosphere (x: vacuum, y: gas).

When the installation location is a vacuum processing chamber A-2 When the formation method is sputtering,
A-2-I-a. The film suction function can be used after the deposited film is formed.
A-2-I-b. A vacuum pump can be used after the deposited film is formed.

A-4 When the formation method is vapor deposition,
A-4x-Ah-a. The suction action of the film can be used during the formation of the deposited film in a vacuum atmosphere (x).
A-4x-Ah-b. A vacuum pump can be used during deposition film formation in a vacuum atmosphere (x).
A-4y-i-a. The suction action of the film can be used after the deposited film is formed in the gas atmosphere (y).
A-4y-i-b. A vacuum pump can be used after deposit film formation in gas atmosphere (y).

B When the installation location is a spare chamber communicating with the vacuum processing chamber B-2 When the formation method is sputtering,
B-2-I-a. The film suction function can be used after the deposited film is formed.
B-2-I-b. A vacuum pump can be used after the deposited film is formed.

B-3 When the formation method is by sublimation,
B-3-A-a. The suction action of the film can be used during the formation of the deposited film.
B-3-a-b. A vacuum pump can be used during deposition film formation.

B-4 When forming method is vapor deposition B-4x-a-a. The suction action of the film can be used during the formation of the deposited film in a vacuum atmosphere (x).
B-4x-Ah-b. A vacuum pump can be used during deposition film formation in a vacuum atmosphere (x).
B-4y-i-a. The suction action of the film can be used after the deposited film is formed in the gas atmosphere (y).
B-4y-i-b. A vacuum pump can be used after deposit film formation in gas atmosphere (y).

DESCRIPTION OF SYMBOLS 1 Vacuum processing apparatus 2 Case 2a Vacuum processing chamber 2b Opening / closing lid 2c Connection part 2d Introduction part 3 Holding mechanism 4 Storage container 5 Electron gun 6 Shutter mechanism 7 Mounting base 10 Sublimation pump 12 Filament 13 Support body 13a Attachment fixing part 13b Fixing Plate 13c Support pillar 14 Support plate 15 Power source 16 Deposition plate 17 Shield plate 17a Inlet 18 Deposition film 19 Cooling means 100 Vacuum processing device 101 Preliminary chamber 101a Indoor deposition wall surface 101c Si-based target 101d Si-based deposition film 101e Second operation means 101h Communication port 102 Housing 102a Vacuum processing chamber 102b Open / close lid 102c Connection portion 102e Second operating means 103 Holding means 104 Mounting table 105 Operating means

Claims (6)

A Si-based material in a solid state which is any one of Si, Si alloy, Si compound, and Si mixture is installed in a vacuum processing chamber or a preliminary chamber communicating adjacent to the vacuum processing chamber, or the vacuum processing chamber, or In the preliminary chamber, the Si-based material is directly or indirectly changed from a solid phase to a vapor phase, and a Si-based deposition film is deposited in at least a part of the vacuum processing chamber or the preliminary chamber, thereby Or evacuate the vacuum processing chamber and the reserve chamber ,
The Si-based material is a wire-like Si-based filament, and the preliminary chamber is a filament storage chamber for storing the Si-based filament, and is heated and sublimated below the melting point of the Si-based filament to be in a gas phase state. And forming the Si-based deposited film on at least a part of the filament storage chamber .   A Si-based material in a solid state which is any one of Si, Si alloy, Si compound, and Si mixture is installed in a vacuum processing chamber or a preliminary chamber communicating adjacent to the vacuum processing chamber, or the vacuum processing chamber, or In the preliminary chamber, the Si-based material is directly or indirectly changed from a solid phase to a vapor phase, and a Si-based deposition film is deposited in at least a part of the vacuum processing chamber or the preliminary chamber, thereby Or evacuate the vacuum processing chamber and the reserve chamber,
  The Si-based material is a Si-based material to be heated that is any one of powder, granules, sheets, or pellets, and the Si-based material to be heated is placed in a storage container that is a boat or a crucible, or the vacuum processing chamber or The Si-based material to be heated in the storage container is heated to a melting point or higher by a heating means provided in one of the preliminary chambers and provided in the vacuum processing chamber or the preliminary chamber to evaporate and evaporate, A vacuum suction method comprising: depositing the Si-based deposited film on at least a part of the substrate or at least a part of the preliminary chamber. The vacuum processing chamber, or the vacuum processing chamber and the spare chamber are in an inert gas, a mixed gas of an inert gas and a reactive gas, or a gas atmosphere that becomes a reactive gas, or in a vacuum atmosphere. , vacuum suction method according to claim 1 or claim 2, characterized in that depositing the Si-based deposited film. An inert gas, a mixed gas of an inert gas and a reactive gas, or a vacuum processing chamber in which a workpiece is processed in a gas atmosphere that becomes a reactive gas or in a vacuum atmosphere, and adjacent to the vacuum processing chamber a vacuum processing apparatus comprising a preliminary chamber communicating, and a vacuum pump to a connected the vacuum processing chamber to the vacuum processing chamber to a vacuum,
An installation section for installing a Si-based material in a solid phase that is any of Si, Si alloy, Si compound, and Si mixture in the vacuum processing chamber or the preliminary chamber;
Gas phase means for directly or indirectly changing the Si-based material installed in the installation part from the solid phase state to the gas phase state,
After depositing the Si-based deposition film in the vacuum atmosphere or depositing the Si-based deposition film in the gas atmosphere at least in a part of the vacuum processing chamber or the reserve chamber by the vapor phase means. , Activate the vacuum pump,
The Si-based material is a wire-like Si-based filament, and the preliminary chamber is a filament storage chamber for storing the Si-based filament, and is heated and sublimated below the melting point of the Si-based filament to be in a gas phase state. And forming the Si-based deposited film on at least a part of the filament storage chamber . An inert gas, a mixed gas of an inert gas and a reactive gas, or a vacuum processing chamber in which a workpiece is processed in a gas atmosphere that becomes a reactive gas or in a vacuum atmosphere, and adjacent to the vacuum processing chamber a vacuum processing apparatus comprising a preliminary chamber communicating, and a vacuum pump to a connected the vacuum processing chamber to the vacuum processing chamber to a vacuum,
An installation section for installing a Si-based material in a solid phase that is any of Si, Si alloy, Si compound, and Si mixture in the vacuum processing chamber or the preliminary chamber;
Gas phase means for directly or indirectly changing the Si-based material installed in the installation part from the solid phase state to the gas phase state,
After depositing the Si-based deposition film in the vacuum atmosphere or depositing the Si-based deposition film in the gas atmosphere at least in a part of the vacuum processing chamber or the reserve chamber by the vapor phase means. , Activate the vacuum pump,
The Si-based material is a Si-based material to be heated that is any one of powder, granules, sheets, or pellets, and the Si-based material to be heated is placed in a storage container that is a boat or a crucible, or the vacuum processing chamber or The Si-based material to be heated in the storage container is heated to a melting point or higher by a heating means provided in one of the preliminary chambers and provided in the vacuum processing chamber or the preliminary chamber to evaporate and evaporate, A vacuum processing apparatus , wherein the Si-based deposition film is deposited on at least a part of the preliminary chamber or at least a part of the preliminary chamber . A sublimation pump that performs vacuum suction in a vacuum processing chamber,
A Si-based filament formed from a Si-based material in a solid state that is any one of Si, Si alloy, Si compound, and Si mixture, a support that supports both ends of the Si-based filament, and a filament through the support A power source that heats and sublimates at a melting point or lower, and a cylindrical body that is installed so that the inner peripheral surface faces around the Si-based filament,
A sublimation pump, wherein the Si-based filament is sublimated through the power source to form a Si-based deposited film on the inner peripheral surface of the cylindrical body and vacuum suction is performed.

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