JP4787636B2 - High pressure processing equipment - Google Patents

Description

  The present invention relates to a high-pressure processing apparatus for processing a substrate, for example, a semiconductor wafer, using a processing fluid containing a supercritical fluid and a film forming raw material.

Along with the high integration of semiconductor devices, development of a technique for embedding a wiring material in a fine pattern having a high aspect ratio is being promoted. As one of the techniques, a fine pattern film forming method using a supercritical fluid as a film forming material medium has been proposed. For example, in order to form a copper (Cu) wiring, a precursor (precursor compound) made of, for example, an organic complex compound containing Cu is dissolved in carbon dioxide (CO ₂ ) in a supercritical state, and this is a reducing agent. A processing fluid to which hydrogen (H ₂ ) is added is supplied to the surface of a semiconductor wafer (hereinafter referred to as “wafer”) to form a Cu film.

  The supercritical state means that when the temperature / pressure of a substance becomes equal to or higher than the value (critical point) specific to the substance, the substance has a characteristic of both gas and liquid. Therefore, if a substance in a supercritical state is used for the medium, it has a density and solubility close to that of a liquid, so that the solubility of the precursor can be maintained higher than that of a gaseous medium, while using a diffusion coefficient close to that of a gas. It is possible to transport the precursor to the wafer more efficiently than the liquid medium. Therefore, in film formation using a processing fluid in which a precursor is dissolved in a supercritical medium, it is possible to perform film formation with high film formation speed and good coverage to a fine pattern (for example, Patent Document 1).

  FIG. 17 shows an example of a system that performs such a film forming method, and shows a simplified high-pressure processing apparatus 1 that supplies a processing fluid to a wafer. The high-pressure processing apparatus 1 includes a stage heater 11 for placing and heating the wafer W, and a processing container 12 surrounding the stage heater 11, and supercritical carbon dioxide and a precursor are contained in the processing container 12. A Cu film is formed on the surface of the wafer W by introducing a processing fluid containing hydrogen as an additive (reducing agent).

  As described above, in the high-pressure processing apparatus 1, a processing fluid having a high pressure, for example, about 12 MPa, is introduced into the processing container 12, so that the processing container 12 can withstand high pressure (a material that does not break even when high tension is applied). For example, it is formed of stainless steel (hereinafter referred to as “SUS”). Further, the temperature of carbon dioxide in the supercritical state introduced into the film formation processing space is about 40 ° C., and the set temperature of the stage heater 11 for heating the wafer W is about 250 to 300 ° C.

  Here, in forming a Cu metal film using carbon dioxide in a supercritical state, the Cu film thickness deposited on the wafer depends on the wafer temperature. FIG. 18 shows the relationship between the wafer temperature and the film thickness of the Cu film. As a result, it is recognized that when the wafer temperature increases, the film thickness of the Cu film increases, and a proportional relationship exists between the two. In the figure, the horizontal axis represents the wafer temperature, the vertical axis represents the Cu film thickness, the ◆ data represents the film formation temperature of 300 ° C., and the square data represents the film formation temperature of 250 ° C.

  As described above, since the influence of the wafer temperature on the film formation is very large, the stage heater 11 for heating the wafer W is required to have extremely good temperature uniformity. Incidentally, the current stage heater 11 has a problem that the temperature uniformity is poor under a high pressure such as a supercritical state. FIG. 19 shows the temperature distribution of the wafer W actually placed on the stage heater 11 in a supercritical state where the carbon dioxide pressure is 12 MPa.

  In the figure, the horizontal axis is the position on the wafer, and when it is 0, it indicates the wafer center, the left vertical axis indicates the wafer temperature, and the right vertical axis indicates the film thickness of the Cu film. In the figure, ◆ is the measured temperature when the heater temperature is set to 300 ° C, and □ is the measured temperature when the heater temperature is set to 250 ° C. It is clear that the temperature tends to be high in the part. The figure also shows the Cu film thickness data when the heater temperature is set to 300 ° C., and the Cu film thickness data when the heater temperature is set to 250 ° C. by Δ. From the figure, it is understood that the film thickness depends on the temperature of the wafer W.

  The reason is considered as follows. First, the processing vessel 12 using a supercritical fluid is made of SUS in order to withstand the pressure for maintaining the supercritical fluid, and has a large thickness, thereby forming a narrow film formation processing space. . As described above, the film forming process space is surrounded by the SUS layer having a small thermal conductivity, and the thickness of the SUS layer is large. Therefore, the way of heat escaping from the film forming process space through the processing container 12 differs depending on the part. When the temperature control is not performed at the bottom of the processing container 12, a hot part and a cold part are formed. As a result, the in-plane temperature difference of the processing container 12 is reflected on the stage heater 11, and uneven heat dissipation of the stage heater 11 occurs. This infers that the in-plane temperature uniformity of the stage heater 11 deteriorates, which is a factor that deteriorates the in-plane temperature uniformity of the wafer W.

  As shown in FIG. 17, the stage heater 11 includes a planar heater portion 13, a support portion 14 that extends downward at the center portion of the heater portion 13, and accommodates a heater power supply line and the like of the heater portion 13. One of the factors is considered to be a mushroom type (T-shaped longitudinal section) formed by That is, the stage heater 11 has a structure in which the support portion 14 is pulled and pressure-sealed with the processing container 12 by the sealing material 15, so that heat easily escapes from the central seal portion to the processing container 12. As a result, the temperature of the central portion of the stage heater 11 becomes lower than that of the peripheral portion. Further, in the above-described seal structure, since the support portion 14 is always pulled downward, the central portion of the stage heater 11 is easily recessed due to the structure, and uneven contact with the wafer W is likely to occur, so that the central portion of the wafer W is generated. It is also considered that one of the factors is that the temperature of the glass becomes lower than that of the peripheral portion. For this reason, it is desired to develop a stage heater 11 having high in-plane temperature uniformity in a supercritical state.

Japanese Patent Laying-Open No. 2005-187879 (FIG. 1, paragraph 0018, paragraph 0019)

  The present invention has been made under such circumstances, and an object thereof is to solve the problem of temperature stability of the stage heater when performing film formation on a substrate using a supercritical fluid, and An object of the present invention is to provide a technique capable of uniforming the temperature in the in-plane direction of the stage heater and performing a film forming process with high in-plane uniformity.

Therefore, the present invention provides a high-pressure processing apparatus for forming a film on a substrate by supplying a processing fluid containing a supercritical fluid and a film-forming raw material into a pressure-resistant vessel.
A stage heater on which the substrate is placed and provided with a heating element;
A heat insulating layer provided on the lower side of the stage heater and having a thermal conductivity smaller than the thermal conductivity of the material of the pressure vessel;
A temperature adjustment layer provided between the heat insulation layer and the bottom portion of the pressure vessel, and provided with a temperature adjustment portion for transferring heat to and from the outside of the pressure vessel. It is characterized by. Here, as the temperature adjusting unit, a flow pipe through which the temperature adjustment medium flows or a heat pipe having one end portion positioned in the flow path of the temperature adjustment medium sent from the outside of the pressure resistant container can be used. Moreover, the said temperature control layer may comprise a part of bottom face part of the said pressure | voltage resistant container instead of being interposed and provided between a heat insulation layer and the bottom face part of the said pressure | voltage resistant container.

Furthermore, the present invention provides a high-pressure processing apparatus for forming a film on a substrate by supplying a processing fluid containing a supercritical fluid and a film-forming raw material into a pressure-resistant vessel.
A stage heater on which the substrate is placed and provided with a heating element;
And a flow path for passing a heat-insulating supercritical fluid provided between the stage heater and the bottom surface of the pressure vessel.

  Here, in this apparatus, a temperature adjusting unit for transferring heat to and from the outside of the pressure vessel is provided so as to be interposed between the flow path of the supercritical fluid and the bottom portion of the pressure vessel. A temperature adjustment layer may be provided. Further, as the temperature adjusting section, a heat pipe in which one end portion is positioned in a flow path through which the temperature adjusting medium flows or in a flow path of the temperature adjusting medium sent from the outside of the pressure resistant container may be used.

  The stage heater includes a planar heater portion in which a heating unit is embedded, and a support portion extending downward from a substantially central portion of the heater portion. The heat-insulating layer having a thermal conductivity smaller than the thermal conductivity of the material of the pressure vessel may be provided, or a part of the bottom surface portion of the pressure vessel, and the flow path of the supercritical fluid The structure in which the heat insulation layer which has heat conductivity smaller than the heat conductivity of the material of the said pressure | voltage resistant container is provided in the site | part which contact | connects may be sufficient. Furthermore, a temperature adjusting means for adjusting the temperature of the supercritical fluid supplied to the flow path of the supercritical fluid may be provided.

  According to the present invention, since the heat insulating layer having a thermal conductivity smaller than the thermal conductivity of the material of the pressure vessel is provided between the stage heater and the bottom portion of the pressure vessel, the heat from the stage heater is reduced. It becomes difficult to transfer heat to the bottom surface side of the pressure vessel, and a state in which heat escapes from a specific part of the stage heater to the pressure vessel side is less likely to occur. In addition, a temperature adjustment layer is provided between the heat insulation layer and the bottom surface of the pressure vessel, and the temperature adjustment is performed so that the temperature of the temperature adjustment layer is maintained at the set temperature by the temperature adjustment unit. The internal temperature is made uniform, and this is reflected on the stage heater through the heat insulating layer. For this reason, unevenness of heat radiation from the stage heater is less likely to occur, and the uniformity of the in-plane temperature of the stage heater is improved. As a result, the in-plane temperature of the substrate becomes stable, and a film forming process with high in-plane uniformity can be performed on the substrate.

  Further, according to another invention of the present invention, by passing a supercritical fluid for heat insulation between the stage heater and the bottom portion of the pressure vessel, gas is introduced between the stage heater and the bottom portion of the pressure vessel. Since the heat insulating layer is formed, heat radiation from the stage heater hardly occurs. For this reason, since the unevenness of heat radiation of the stage heater is less likely to occur, the in-plane temperature of the substrate becomes stable, and a film forming process with high in-plane uniformity can be performed on the substrate.

  Hereinafter, the high-pressure processing apparatus according to the present invention will be described with reference to FIG. In FIG. 1, reference numeral 2 denotes an apparatus main body. The apparatus main body 2 mounts a pressure-resistant frame member 20 constituting a side surface and a bottom surface, an upper lid 21 that closes an upper opening of the pressure-resistant frame member 20, and a wafer W that is a substrate. And a mounting table 3 for mounting. The pressure-resistant frame member 20 and the upper lid 21 are made of stainless steel (hereinafter referred to as “SUS”) that can withstand a pressure for maintaining a supercritical processing fluid described later. The thermal conductivity of this SUS is 16.5 W / m · K at 100 ° C. In addition to SUS, for example, carbon steel, titanium, Hastelloy (registered trademark of Haynes International, USA) and Inconel (registered trademark of USA Special Metal) may be used. A ring groove 22 is formed on the pressure frame material 20 side at a portion where the upper surface of the pressure frame material 20 and the lower surface of the upper lid 21 are in contact, and an O-ring 23 is accommodated in the ring groove 22. The adhesion between the pressure-resistant frame member 20 and the upper lid 21 is enhanced. A seal plate 24 for separating a piston, which will be described later, from the atmosphere, is provided below the mounting table 3.

  The mounting table 3 is connected to a piston body 26 through a piston neck 25 penetrating the seal plate 24. A hydraulic cavity 27 is formed below the piston body 26, and a hydraulic fluid system (not shown) is connected to the hydraulic cavity 27. The amount of liquid supplied into the hydraulic cavity 27 is adjusted by the liquid fluid system. A pneumatic cavity 28 is formed between the seal plate 24 and the piston body 26, and a pneumatic fluid system (not shown) is connected to the pneumatic cavity 28. The amount of gas supplied into the pneumatic cavity 28 is adjusted by the gas-fluid system. Thus, in this example, the piston body 26 is moved up and down by adjusting the amount of liquid supplied into the liquid cavity 27 and the amount of gas supplied into the atmospheric pressure cavity 28. As the piston body 26 moves up and down, the mounting table 3 moves up and down. Here, ring grooves 24 a and 24 b are formed on the seal plate 24 side between the seal plate 24 and the pressure-resistant frame member 20 and between the seal plate 24 and the piston neck 25, respectively. O-rings 24c and 24d are accommodated in 24b, respectively, to improve the adhesion between them. Further, a ring groove 26a is formed on the piston body 26 side between the piston body 26 and the pressure resistant frame member 20, and an O-ring 26b is accommodated in the ring groove 26a. It is increasing.

  Here, the mounting table 3 is configured by laminating the stage heater 4, the heat insulating layer 51, and the temperature adjustment layer 53 in this order from above on the upper side of the mounting table main body 31. A space surrounded by the mounting table 3, the pressure-resistant frame material 20, and the upper lid 21 is a film-forming treatment space F. By the mounting table 3, the pressure-resistant frame material 20 and the upper lid 21, a supercritical fluid and a film-forming raw material are formed. A pressure-resistant container that performs a film forming process on the wafer W is configured by a processing fluid including Therefore, the mounting table main body 31 constitutes a part of the bottom surface portion of the pressure-resistant container in the scope of claims, and therefore the mounting table main body 31 can withstand the pressure for maintaining the supercritical processing fluid described later. Thus, the thickness is set to about 10 cm, for example.

  A planar stage heater 4 is provided at the central portion of the upper portion of the mounting table 3. A concave portion 41 for dropping the wafer W is provided on the upper surface of the stage heater 4 as shown in FIG. Is formed. The recess 41 has a size substantially the same as or slightly larger than the wafer W, and the depth of the recess 41 is formed to be about 0.5 mm. A vacuum chuck layer (not shown) is formed on the mounting surface of the wafer W in the concave portion 41 so that the wafer W is vacuum-sucked. Further, instead of vacuum suction, an electrostatic chuck that electrostatically attracts can be used.

  The stage heater 4 is made of, for example, SUS, which is the same material as the pressure vessel, and includes a sheath heater 42 that forms a spiral heating element and a distal end portion as shown in FIGS. 2 and 3, for example. And a thermocouple 43 provided so as to extend horizontally in the stage heater 4 so as to be positioned at, for example, the center of the stage heater 4. The sheath heater 42 is disposed so that the amount of heat generated per unit area (heat generation wattage) is substantially uniform over the entire surface of the stage heater 4 so that the center region of the stage heater 4 is not sparser than the peripheral region.

  For example, as shown in FIG. 3, such a stage heater 4 is formed so as to sandwich the sheath heater 42 and the thermocouple 43 from above and below by an upper member 4A and a lower member 4B each made of SUS. The thickness L1 of the 41 portion is set to about 10 mm. A Peltier element may be used instead of the sheath heater 42, or a resistance temperature detector may be used instead of the thermocouple 43.

  The mounting table 3 is provided with a heat insulating layer 51 on the lower side of the stage heater 4 so as to surround the lower surface and the side surface of the stage heater 4. Since this heat insulating layer 51 is used to thermally shut off the pressure vessel 2 and the stage heater 4, a material having a lower thermal conductivity than the pressure vessel 2, for example, quartz (quartz glass: thermal conductivity of 100 ° C. 1.9 W / m · K) is used. In addition to quartz, for example, alumina ceramics may be used. Further, as shown in FIGS. 2 and 3, for example, a circular recess 52 for accommodating the stage heater 4 is formed on the upper surface of the heat insulating layer 51, and the thickness L2 of the recess 52 portion of the heat insulating layer 51 is, for example, It is comprised about 1 mm-5 cm.

  Further, the mounting table 3 is provided with a temperature adjustment layer 53 on the lower side of the heat insulating layer 51 so as to surround the lower surface and the side surface of the heat insulating layer 51. For example, as shown in FIGS. 2 and 3, a circular recess 54 for accommodating the heat insulating layer 51 is formed on the upper surface of the temperature adjustment layer 53. As shown in FIG. 3, a temperature control flow path 55 that constitutes a temperature adjustment portion formed in a spiral shape is embedded. The temperature control channel 55 is made of, for example, a 1/4 to 1/2 inch stainless steel pipe. The temperature adjusting unit is for transferring heat to and from the outside of the pressure vessel, and heat may be supplied from the outside of the pressure vessel, or heat may be supplied to the outside of the pressure vessel. May be released.

  Such a temperature adjustment layer 53 is made of a material having the same or larger thermal conductivity as that of the pressure vessel, such as SUS or Al. Here, Al is a preferable material having a thermal conductivity as high as 240 W / m · K at 100 ° C., but is not limited to this, and Cu (thermal conductivity is 350 to 420 W / m · K), aluminum nitride (AlN: A thermal conductivity of 150 to 280 W / m · K), silicon carbide (SiC: thermal conductivity of 200 to 300 W / m · K), or a composite thereof may be used.

  For example, as shown in FIG. 3, the temperature adjustment layer 53 is formed so as to sandwich the temperature adjustment channel 55 from above and below by the upper member 53 </ b> A and the lower member 53 </ b> B. L3 is preferably about 10 mm to 5 cm, for example, and is set to about 20 mm, for example. The thickness L4 of the peripheral region of the temperature adjustment layer 53 is set to about 10 mm, for example.

  As shown in FIG. 1, two sealing devices 32 and 33 that partition the high-pressure atmosphere and the air atmosphere are formed on the lower surface portion (the bottom surface portion of the sealed container) of the mounting table 3. The lead wire of the sheath heater 42 and the other end side of the thermocouple 43 of the stage heater 4 are housed in a common housing 44 and provided to extend downward at a position near the peripheral edge of the stage heater 4, for example. The heat insulating layer 51, the temperature adjusting layer 53, and the mounting table main body 31 are connected to the sealing device 32. The temperature controller 46 adjusts the temperature of the sheath heater 42 based on the detected temperature value of the thermocouple 43 to heat the stage heater 4. Configured to control. In FIG. 2, 51a and 53a are holes provided in the heat insulation layer 51 and the temperature adjustment layer 53, respectively, through which the housing 44 passes.

  The temperature adjustment channel 55 of the temperature adjustment layer 53 is provided so as to extend downward at a position near the peripheral edge of the temperature adjustment layer 53, and is connected to the sealing device 33 via the mounting table body 31. And it is connected to the chiller unit 56 provided outside the pressure vessel through this sealing device 33. As the temperature control medium, Galden (registered trademark of Ikuno Solvay Solexis) or Florinart (registered trademark of 3M USA) is used. The temperature control medium set to the same or higher temperature, for example, about 40 ° C. to 90 ° C. and adjusted to a preset temperature is supplied to the temperature control flow channel 55. In this way, heat is transferred to and from the outside of the pressure vessel in the temperature adjustment flow path 55 which is a temperature adjustment unit provided in the temperature adjustment layer 53. Further, the mounting table 3 is provided with lifter pins 35 configured to be movable up and down by, for example, a three-point support type lifting mechanism 34 for delivering the wafer W to the mounting table 3.

  A spacer 36 is interposed between the lower surface portion of the upper lid 21 and the upper surface portion of the pressure-resistant member 20. A ring groove 26 is formed on the pressure frame material 20 side at a portion where the upper surface of the pressure frame material 20 and the lower surface of the spacer 36 are in contact, and an O-ring 27 is accommodated in the ring groove 26. The adhesion between the pressure-resistant frame member 20 and the spacer 36 is enhanced. Further, a ring groove 28 is formed on the mounting table 3 side at a portion where the lower surface of the spacer 36 and the upper surface of the mounting table 3 (mounting table main body 31) are in contact with each other. 29 is accommodated, and the adhesion between the mounting table 3 and the spacer 36 is enhanced.

  Further, inside the upper lid 21, as shown in FIG. 1, a supply path 60 for supplying a processing fluid containing a supercritical fluid as a medium and a film forming raw material into the film forming processing space F, A discharge path 61 for discharging the processing fluid from the film processing space F is formed. In this example, the processing fluid flowing through the supply path 60 is from one end side to the other end side of the wafer W (FIG. 1). It flows from the left side to the right side in the inside and is discharged through the discharge path 61.

  A supply pipe 62 and a discharge pipe 63 are connected to the supply path 60 and the discharge path 61, respectively, and a circulation path 64 is formed by the supply pipe 62 and the discharge pipe 63. Discharge valves V1 and V2, a circulation / heating / cooling unit 65, and a valve V3 are connected to the circulation path 64 in this order from the discharge pipe 63 side. A branch pipe 66 is formed between the discharge valves V1 and V2, and a back pressure valve V4 and a discharge portion 67 are connected to the branch pipe 66. The discharge part 67 includes a separation / recovery unit, a recovery valve, a liquid recovery part, and a gas discharge part (not shown), and a vacuum pump (not shown) is further provided as necessary.

A branch pipe 68 and a branch pipe 69 are connected to the supply pipe 62. A raw material mixer / heater 100 is connected to the branch pipe 68 via an introduction valve V7. A reducing agent mixing / heating device 110 is connected to the branch pipe 69 via an introduction valve V12. A precursor supply unit 101 is connected to the raw material mixer / heater 100 via a valve V8. The precursor supply unit 101 includes a precursor (precursor compound) made of, for example, an organic complex compound containing Cu as a film forming raw material, for example, a metal raw material storage tank 102 and a metal raw material pressurizer 103 in which Cu (hfac) ₂ is stored. Composed. A reducing agent supply unit 111 is connected to the reducing agent mixing / heating device 110 via a valve V11. The reducing agent supply unit 111 includes a reducing agent storage tank 112 in which, for example, hydrogen (H ₂ ) as a reducing agent is stored.

  Further, the raw material mixing / heating device 100 and the reducing agent mixing / heating device 110 are connected to a medium storage tank 120 storing carbon dioxide, a supply source valve V5, a cooler 121, and a pressurizer 122 from the upstream side. ing. As the medium storage tank 120, a carbon dioxide cylinder or the like can be used. In addition, a processing fluid such as a medium flowing in the pipe, for example, carbon dioxide or carbon dioxide in which a raw material is dissolved is maintained at a temperature exceeding 30 ° C. for maintaining a supercritical state, for example, 40 ° C. To prevent the temperature from fluctuating greatly, a pipe or a valve extending from the downstream side of the pressurizer 122 to the discharge unit 67 is wound with a heater, a heat insulating material, or the like so that the temperature can be appropriately controlled. ing. Further, a transfer port 2 </ b> A for carrying the wafer W in and out of the pressure resistant container 2 is formed on the side surface of the pressure resistant frame member 20.

  Next, in the above-described high-pressure processing apparatus, the operation until the wafer W is mounted on the mounting table 3 in the pressure-resistant container constituted by the pressure-resistant frame member 20, the upper lid 21, and the mounting table 3 will be described. In the state shown in FIG. 4A, the mounting table 3 is in the closed position, that is, the mounting table 3 and the spacer 36 are in close contact via the O-ring 29 and are surrounded by the upper lid 21 and the mounting table 3. The film processing space F is in an empty state. First, as shown in FIG. 4B, the mounting table 3 is lowered to the loading position by the piston body 26 (not shown). Thereafter, a wafer W as a substrate is carried into the pressure-resistant container through a transfer port 2A from a load lock chamber (not shown) in a vacuum atmosphere by a transfer arm (not shown).

  Subsequently, as shown in FIG. 4C, the lifter pins 35 are moved up to a position where the wafer W is transferred by the elevating mechanism 34, whereby the wafer W is raised and separated from the transfer arm (not shown). Is withdrawn from the pressure vessel. After the wafer W is transferred to the lifter pins 35 in this way, the lifter pins 35 are lowered to transfer the wafer W to the mounting position of the wafer W formed by the recess 41 of the stage heater 4 as shown in FIG. Then, the wafer W is vacuum-adsorbed on the stage heater 4 by a vacuum chuck layer (not shown). Thereafter, as shown in FIG. 5B, the mounting table 3 is raised by the piston body 26 (not shown), and the mounting table 3 and the spacer 36 are brought into close contact with each other via the O-ring 29.

  Next, a series of film forming processes using the high-pressure processing apparatus of the present invention will be described with reference to FIG. First, the wafer W is loaded into the pressure-resistant container according to the procedure described above, and the inside of the film formation processing space F is evacuated using the discharge unit 67 (step S1). On the other hand, the stage heater 4 in the mounting table 3 is turned on in advance, and the surface of the mounting table 3 is set to a temperature of 200 ° C. to 350 ° C., preferably 250 ° C. to 300 ° C., for example. Further, a temperature control medium set to 40 ° C. to 90 ° C., preferably 40 ° C. to 70 ° C., is passed through the temperature adjustment layer 53 by the chiller unit 56.

  Next, the supply valve V5 and the introduction valve V7 are opened, and a medium (carbon dioxide) heated to a predetermined temperature, for example, 40 ° C., is introduced into the film formation processing space F through the raw material mixing / heating device 100, whereby The pressure in the film processing space F is increased to about the pressure in the medium storage tank 120. Thereafter, in order to introduce carbon dioxide having a pressure exceeding the pressure inside the medium storage tank 120, the carbon dioxide pressurized by the pressurizer 122 is introduced into the film forming treatment space F through the cooler 121. Also in this case, by passing the raw material mixing / pressurizing device 100, the carbon dioxide to be introduced is pressurized to a predetermined processing pressure, for example, 12 MPa, while maintaining a predetermined temperature, and in a supercritical state. Carbon dioxide (supercritical fluid) is obtained. At this time, the discharge valve V1 is opened, and a predetermined pressure is maintained by pressure control of the back pressure valve V4 (step S2).

  This process is an example in which carbon dioxide having a pressure higher than the pressure inside the medium storage tank 120 is introduced into the pressure vessel. The medium storage tank 120 is provided with a pressurizing unit, and the carbon dioxide is supplied at a pressure higher than the processing pressure. In the case where it can be supplied, instead of the cooler 121 and the pressurizer 122, a path that passes only the raw material mixing / pressurizer 100 through a pressure reducing valve may be used.

After the metal raw material pressurizer 103 is operated, the valve V8 is immediately opened, and the liquid metal raw material is mixed with the supercritical carbon dioxide having a predetermined pressure through the cooler 121 and the pressurizer 122 by the raw material mixing / heating device 100. . Thereby, the process fluid which mixed the metal raw material with the supercritical fluid of predetermined temperature, for example, 40 degreeC is produced | generated. This processing fluid can be continuously supplied to the pressure vessel through the introduction valve V7 by operating the pressurizer 122 and the metal raw material pressurizer 103 continuously. Here, as the liquid metal raw material, a precursor of Cu (hfac) ₂ or the like dissolved in an organic solvent such as alcohol can be used.

  Gaseous reducing agent In this example, when mixing hydrogen, a reducing agent adjusted to a predetermined pressure, for example, 0.9 MPa, is mixed with supercritical carbon dioxide through the reducing agent mixing / heating device 110, and the processing fluid is mixed. Generate. This processing fluid is supplied to the film forming processing space F through the introduction valve V12 (step S3). When a liquid reducing agent such as alcohol is used, it is possible to generate a processing fluid by applying pressure and mixing in the same manner as the liquid metal raw material.

  Then, the processing fluid flowing through the supply path 60 enters the film forming processing space F, flows from one end side of the wafer W to the other end side (from the left side to the right side in FIG. 1), and passes through the discharge path 61. Discharged. At this time, the valve V2 and the valve V3 of the circulation path 64 are opened, and the processing fluid is circulated by the circulation / heating / cooling unit 65, thereby performing the film formation process for a predetermined time. On the surface of the wafer W thus placed on the mounting table 3, a reaction shown in the following formula (1) occurs, and the precursor is thermally decomposed, whereby a Cu film is formed on the surface of the wafer W.

Cu (hfac) ₂ + H ₂ → Cu + 2H (hfac) (1)
After the Cu film is formed on the wafer W, the valves V2, V3, the introduction valve V7, and the introduction valve V12 are closed to stop the supply of the processing fluid. For the metal raw material, the valve V8 is closed and the metal raw material pressurizer 103 is stopped to stop the mixing with the processing fluid. Similarly, the supply of the reducing agent to the processing medium is stopped by closing the valves V9 and V11 (step S4).

  Then, the discharge valve V1 is opened, the back pressure valve V4 is opened by lowering the set pressure, and the processing fluid in the film formation processing space F is discharged by the discharge unit 67 (step S5). At this time, carbon dioxide is discharged from the gas discharge portion in the discharge portion 67. Further, if a separation / purification / condenser for carbon dioxide is provided at the end of the gas discharge section, carbon dioxide can be reused. As described above, the wafer W is discharged from the pressure vessel into a load lock chamber in a vacuum atmosphere (not shown) by performing a reverse operation to the series of operations for placing the wafer W on the mounting table 3 in the pressure vessel. (Step S6). The film forming process is performed on the subsequent wafer W in the same manner.

  As described above, in the above-described apparatus, the pressure-resistant container is formed by the pressure-resistant frame member 20, the upper lid 21, and the mounting table 3 around the film-forming process space F. In the film-forming process, the heat from the stage heater 4 is formed. Radiates heat through the heat insulating layer 51 and the temperature adjusting layer 53 to the mounting table body 31 forming the bottom surface of the pressure vessel. At this time, according to the above-described embodiment, the stage heater 4 is covered with the heat insulating layer 51 made of a material having a thermal conductivity smaller than that of the pressure vessel. 4 and the bottom surface of the pressure vessel (mounting table main body 31) are thermally blocked, and the heat of the stage heater 4 is difficult to transfer to the pressure vessel side. This makes it difficult for heat to escape from a specific location of the stage heater 4, so that uneven heat dissipation from the stage heater 4 to the heat-resistant container can be prevented. As a result, the in-plane temperature of the stage heater 4 is uniform. Can increase the sex.

  Further, in this example, a temperature adjustment layer 53 is provided between the stage heater 4 and the mounting table main body 31, and the temperature adjustment medium 53 is passed through the temperature adjustment layer 53, so that heat can be transferred between the outside of the pressure-resistant container. The temperature is adjusted so that the temperature of the temperature adjustment layer 53 can be maintained at the set temperature by giving and receiving. As a result, the temperature in the in-plane direction of the temperature adjustment layer 53 is uniformed, so that the heat insulating layer 51 in contact with the temperature adjustment layer 53 is also less likely to have a gradient in the temperature in the in-plane direction. Accordingly, since the in-plane temperature of the heat insulating layer 51 becomes uniform, this is reflected in the stage heater 4, and the heat from the stage heater 4 flows toward the heat insulating layer 51 uniformly in the in-plane direction. In this way, uneven heat dissipation of the stage heater 4 can be further prevented, so that the in-plane temperature uniformity of the stage heater 4 can be further improved. As a result, the in-plane uniformity of the wafer temperature is also increased. As a result, a film forming process with high in-plane uniformity can be performed on the wafer W, and a high in-plane uniformity of the Cu film thickness can be obtained. Can do.

  Furthermore, in the above-described example, the stage heater 4 has a planar shape, so that heat escape from the stage heater 4 is smaller than that of a conventional mushroom type stage heater, and the shape of heat dissipation is uniform in the plane. It is easy to become. Furthermore, since the sheath heater 42 embedded in the stage heater 4 is provided so that the heat generation wattage per unit area is substantially uniform in the plane, the heat generation amount is aligned in the plane, and the stage heater 4 In-plane uniformity of temperature is higher.

  Further, since the lead wire of the sheath heater 42 and the thermocouple 43 are drawn downward on the peripheral edge of the stage heater 4, provision of a housing 44 for storing them changes the way in which the heat escapes in the vicinity. Even if the case 44 is assumed, the position where the housing 44 is provided is a part of the peripheral edge of the stage heater 4, so that the lead wire of the sheath heater 42 and the thermocouple 43 are drawn downward from the center of the stage heater 4. Compared to the case, the influence on the in-plane temperature uniformity is small. Further, in this example, since only the conductor wire of the sheath heater 42 and the thermocouple 43 are sealed by the sealing device 32, the stage heater 4 is pulled as in the case of pressure sealing by pulling the supporting part of the conventional mushroom type stage heater. In this respect, it is difficult to cause uneven contact between the stage heater 4 and the wafer W, so that deterioration of the in-plane uniformity of the temperature of the wafer W can be prevented. Can do.

Next, another example of the present invention will be described with reference to FIG. This example is different from the apparatus shown in FIG. 1 in that a heat pipe 71 forming a temperature adjustment unit is embedded in a spiral shape instead of the temperature adjustment channel 55 of the temperature adjustment layer 53, and a thermocouple as a temperature detection means. 72 is provided so as to extend horizontally in the temperature adjustment layer 53 so that the front end portion is located at substantially the center of the temperature adjustment layer 53.
The heat pipe 71 is sealed at both ends, and a porous body made of metal, metal felt, or the like is attached to the inner wall, and a volatile liquid (working fluid) in a tube made of metal having a vacuum inside, for example, copper. Is configured to be enclosed in a small amount. When one end of the heat pipe 71 is heated, the working fluid evaporates and moves to the other end side, and then is refluxed through the porous body to transport heat.

  One end side of the heat pipe 71 and the thermocouple 72 extend downward, for example, at the peripheral edge of the temperature adjustment layer 53, and are connected to the lower side of the mounting table body 31 via a seal device 73. Then, one end side of the heat pipe 71 is connected to a temperature control medium inside the temperature control medium storage tank 74 provided outside the apparatus main body 2 via the sealing device 73, whereby one end side of the heat pipe 71 is connected to the pressure vessel. It is located in the flow path of the temperature control medium sent from the outside. The thermocouple 72 is connected to a temperature controller 75 via a sealing device 73. A chiller unit 76 is connected to the temperature control medium storage tank 74 so that the temperature control medium storage tank 74 is supplied with a temperature control medium such as Galden or Florinart adjusted to a predetermined temperature, for example, 40 ° C. to 90 ° C. It has become. The temperature controller 75 outputs a command for adjusting the temperature of the temperature control medium to the chiller unit 76 based on the temperature detection value of the thermocouple 72, and thus the temperature control medium having a predetermined temperature is stored in the temperature control medium storage tank 74. It is configured to be supplied.

  In this example, when the temperature of the temperature adjustment layer 53 becomes equal to or lower than the set temperature, the heat of the temperature adjustment medium in the temperature adjustment medium storage tank 74 flows to the temperature adjustment layer 53 via the heat pipe 71, and the temperature of the temperature adjustment layer 53 is set. When the temperature is higher than the temperature, heat flows from the heat pipe 71 toward the temperature control medium in the temperature control medium storage tank 74. Then, the temperature of the temperature adjustment layer 53 is detected by the thermocouple 72 so that the temperature of the temperature adjustment layer 53 is maintained within the set temperature range, and the temperature of the temperature adjustment medium is adjusted by the chiller unit 76 via the temperature controller 75. It is supposed to be.

  In such a configuration, the heat adjustment layer 53 is provided with the heat pipe 71 and the thermocouple 72 and is controlled so that the temperature of the temperature adjustment layer 53 falls within the set temperature range. The surface becomes more uniform in the plane, and in the same manner as in the example shown in FIG. 1, the in-plane uniformity of the heat radiation from the stage heater 4 to the pressure vessel can be increased, and the in-plane uniformity of the temperature of the stage heater 4 Will improve. For this reason, since the uniformity of the in-plane temperature of the wafer W is increased, it is possible to perform the film forming process with high in-plane uniformity on the wafer W, and to ensure a high in-plane uniformity with respect to the film thickness of the Cu film. it can.

  Next, another example of the present invention will be described with reference to FIG. This example is different from the apparatus shown in FIG. 1 in that the temperature adjustment layer 53 is provided between the heat insulation layer 51 and the mounting table body 31 instead of being provided between the heat insulation layer 51 and the lower surface of the heat insulation layer 51. A mounting table main body 31 is provided so as to cover the periphery of the side surface, and the temperature adjustment layer is configured by the mounting table main body 31 that forms a part of the bottom surface portion of the pressure vessel, and the heat pipe 77 that forms the temperature adjustment unit on the mounting table main body 31. It is that a plurality of them are buried. The plurality of heat pipes 77 are provided radially inside the mounting table main body 31 as shown in FIG. The heat pipe 77 may be provided in a lattice shape. Further, an annular temperature control channel 78 is formed in the peripheral region inside the mounting table main body 31, and one end side of each heat pipe 77 is positioned in the temperature control channel 78.

  The temperature control channel 78 extends downward on the periphery of the mounting table body 31, extends outward from the apparatus body 2, and is connected to the chiller unit 79. In the chiller unit 79, a temperature adjusting medium such as Galden or Fluorinert is adjusted to a predetermined temperature, for example, 40 ° C. to 90 ° C. and supplied to the temperature adjusting channel 78. In FIG. 8B, reference numeral 80 denotes a temperature control medium supply path from the chiller unit 79 to the temperature control flow path 78, and 81 denotes a temperature control medium discharge path from the temperature control flow path 78 to the chiller unit 79. A partition 82 is provided between these connection portions of the temperature control flow path 78, and the temperature control medium supplied from the chiller unit 79 via the supply path 80 flows through the temperature control flow path 78 and is a discharge path. The temperature control medium that has been smoothly discharged from 81 and thus not separated from the discharge path 81 is not mixed with the supplied temperature control medium. In FIG. 8B, reference numeral 31 a denotes a hole formed in the mounting table main body 31 for passing the housing 44 from the stage heater 4.

  In this example, since the mounting table main body 31 is provided outside the heat insulating layer 51, the heat from the stage heater 4 is dissipated to the mounting table main body 31 side (the bottom surface side of the pressure vessel) through the heat insulating layer 51. However, at this time, the mounting table main body 31 acts as a temperature adjustment layer, and heat is transferred by the heat pipe 77 so that the temperature of the mounting table main body 31 becomes the same as the temperature of the temperature control medium. As a result, in the bottom surface portion of the pressure vessel, the in-plane temperature uniformity is increased without generating a cold region and a warm region, so that the heat escape from the stage heater 4 to the pressure vessel becomes uniform in the surface, Similar to the example shown in FIG. 1, the in-plane uniformity of the temperature of the stage heater 4 is improved. For this reason, since the uniformity of the in-plane temperature of the wafer W is increased, the film forming process can be performed with high in-plane uniformity, and high in-plane uniformity can be ensured with respect to the film thickness of the Cu film.

  Also in this example, similarly to the example shown in FIG. 7, when the mounting table main body 31 is provided with a thermocouple, and the temperature of the mounting table main body 31 falls below the set temperature, the heat pipe 77 from the temperature control medium in the temperature control medium storage tank. When the temperature of the mounting table main body 31 becomes equal to or higher than the set temperature, heat flows from the heat pipe 77 toward the temperature control medium of the temperature control medium storage tank. The temperature of the temperature control medium may be adjusted by the chiller unit based on the temperature information from the thermocouple so that the temperature of the temperature is maintained within the set temperature range.

  Next, still another example of the present invention will be described with reference to FIG. This example differs from the apparatus shown in FIG. 1 in that a supercritical fluid for heat insulation is provided between the stage heater 4 and the mounting table body 31 instead of providing a solid heat insulation layer 51 and a temperature adjustment layer 53. This is because a flow path for allowing flow is formed, and a heat insulating layer is formed by this supercritical fluid. Specifically, a plurality of stage heaters 4 are placed on the mounting table body 31 so that the lower surface and the side surface of the stage heater 4 are covered with the mounting table body 31 through gaps of about 1 to 20 mm and 1 to 20 mm, respectively. Thus, a gap of a predetermined size is formed between the stage heater 4 and the mounting table main body 31, and a supercritical fluid for heat insulation flows through the gap. It becomes the flow path 84 to do.

  A supply path 85 for supplying a heat-insulating supercritical fluid to the flow path 84 is formed in the upper lid 21 and the mounting table body 31. The supply path 85 extends, for example, to the lower side of the upper lid 21 and the mounting table body 31 and bends toward the center of the stage heater 4 on the lower side of the stage heater 4, and on the lower side of the stage heater 4. The flow path 84 is connected. At this time, the supply path 85 is branched and branched at the lower side of the central portion of the stage heater 4 so that the supercritical fluid is supplied to a plurality of locations of the flow path 84 formed on the lower surface side of the stage heater 4. Further, the tip of each supply path 85 is connected to the flow path 84.

  As the supercritical fluid for heat insulation, for example, carbon dioxide in a supercritical state whose temperature is adjusted to 40 ° C. to 90 ° C. is used. For example, the pressurizer is connected to the supply path 85 via a valve V13 and a heater 86. 122, the cooler 121, the valve V5, and the medium storage tank 120 are connected to supply the temperature-controlled supercritical carbon dioxide. When the supercritical carbon dioxide whose temperature is adjusted is supplied to the supply path 85, the supercritical fluid flows from the lower surface side to the side surface side of the stage heater 4 through the flow path 84. The film flows into the film forming process space F and is discharged via the discharge path 61.

  In such a configuration, since the stage heater 4 is levitated from the mounting table main body 31, movement of heat from the stage heater 4 to the mounting table main body 31 is suppressed. Further, since carbon dioxide in a supercritical state has a very low thermal conductivity of 0.08 W / m · K at a temperature of 40 ° C. and a pressure of 12 MPa, it is superb between the stage heater 4 and the mounting table body 31. When carbon dioxide in a critical state is passed, this acts as a heat insulating layer, and further, heat transfer from the stage heater 4 to the mounting table body 31 is suppressed.

  In this way, by passing carbon dioxide in a supercritical state having a very low thermal conductivity between the stage heater 4 and the mounting table main body 31, a part of the bottom portion of the stage heater 4 and the pressure vessel can be obtained. Since the mounting table main body 31 is thermally cut off, it is difficult for heat from a specific part of the stage heater 4 to escape toward the bottom surface side of the pressure vessel, and the temperature of the stage heater 4 is within the plane. Uniformity can be achieved. For this reason, since the uniformity of the in-plane temperature of the wafer W is increased, the film forming process can be performed with high in-plane uniformity, and high in-plane uniformity can be ensured with respect to the film thickness of the Cu film. Further, by passing carbon dioxide in a supercritical state between the stage heater 4 and the mounting table body 31, it is possible to suppress the wraparound of the supercritical fluid that is the processing fluid and the raw material gas into the flow path 84. . As a result, it is possible to prevent Cu from adhering to the side surface and the back surface side of the stage heater 4.

  Further, in this example, as shown in FIG. 10, for example, the flow region of the processing fluid and the flow region of the supercritical fluid for heat insulation may be provided separately. In the example shown in FIG. 10, the heat-conducting supercritical fluid discharge paths 87 and 87 are formed outside the film formation processing space F so that the flow areas of both are divided. For example, the discharge paths 87 and 87 are formed inside the upper lid 21 so as to be connected to a flow path 84 formed between the side peripheral surface of the stage heater 4 and the mounting table main body 31. In this way, since the mixing of the processing fluid as the film forming raw material and the heat insulating supercritical fluid does not occur in the film forming processing space F, the film forming process with higher accuracy can be performed.

  Next, still another example of the present invention will be described with reference to FIG. This example is different from the apparatus shown in FIG. 9 in that the stage heater 88 has a mushroom shape with a T-shaped cross section. First, the stage heater 88 will be described. The heater portion 88a includes a circular flat plate-shaped heater portion 88a made of SUS and a support portion 88b extending downward from the lower surface side central portion of the heater portion 88a. The sheath heater 89 and the thermocouple 90 are embedded through the inside of the support member 88b. In this example, similarly to the example shown in FIG. 9, the lower surface and the side surface of the stage heater 88 are configured to be covered with the mounting table body 31 via a gap, and the supply path is connected to the flow path 91 formed by the gap. A supercritical fluid for heat insulation is supplied through 85. In this example, a part of the supply path 85 protrudes to the outside of the mounting table main body 31 and is connected to the flow path 91 in the vicinity of the lower end of the support portion 88b. However, the supply path 85 is increased by increasing the thickness of the mounting table main body 31. May be formed inside the mounting table main body 31. The lower end side of the mounting table main body 31 and the support portion 88b of the stage heater 88 is connected via O-rings 92a and 92b provided on the mounting table main body 31 side.

  Also in this example, the stage heater 88 and the mounting table main body 31 are thermally moved by passing carbon dioxide in a supercritical state having a very low thermal conductivity between the stage heater 88 and the mounting table main body 31. Therefore, the in-plane uniformity of the temperature of the stage heater 88 can be achieved, and a film forming process with high in-plane uniformity can be performed on the wafer W. High in-plane uniformity can be ensured. Further, by increasing the length of the support portion 88b of the stage heater 88 to, for example, about 10 cm, it is possible to suppress the movement of heat from the heater portion 88a to the bottom surface side of the pressure vessel (the lower side of the mounting table main body 31). .

  Further, in the example shown in FIG. 12, the support part 93b of the mushroom-type stage heater 93 is shortened to, for example, about 5 cm in the example shown in FIG. A heat insulating layer 94 formed of a material having a low thermal conductivity such as the above is provided. In this example, since the support portion 93 b is short, the supply path 85 is formed inside the mounting table main body 31. Other configurations are the same as the example shown in FIG.

  In this way, even if the length of the support portion 93b is short, it is possible to suppress the movement of heat from the heater portion 93a to the bottom surface side of the pressure vessel (the lower side of the mounting table main body 31). In-plane uniformity of the temperature of the stage heater 93 can be improved. The heat insulating layer 94 may be formed of a plastic such as PEEK (registered trademark of Victrex) or TORLON (registered trademark of Solvay Advanced Polymers). Moreover, since the lower end side of the support part 93b contacts the mounting base main body 31, and stress is applied, it is preferable to comprise from SUS.

  Further, the example shown in FIG. 13 is the same as the part shown in FIG. In addition, a heat insulating layer 95 formed of a material having a low thermal conductivity such as quartz glass is provided on the surface of the mounting table main body 31 facing the side surface of the support member 88b. The other configuration is shown in FIG. Similar to the example. In this way, since the heat insulating layer 95 is provided between the stage heater 88 and the mounting table body 31, the heat from the stage heater 88 to the bottom surface side of the pressure vessel (the lower side of the mounting table body 31). The movement can be suppressed, and the in-plane uniformity of the temperature of the stage heater 88 can be further enhanced.

  In the above, the mounting table main body 31 may be configured so as to function as a temperature adjusting layer by embedding a temperature adjusting unit therein. Such an example will be described with reference to FIG. In the mounting table main body 31 of this example, a plurality of first heat pipes 96a are embedded so as to face the heater portion 88a of the stage heater 88, and so as to face the support portion 88b of the stage heater 88. A plurality of second heat pipes 96b are embedded. The first heat pipe 96a and the second heat pipe 96b form a temperature adjusting unit, and are provided, for example, radially inside the mounting table main body 31 like the heat pipe shown in FIG. An annular first temperature control flow path 97a is formed at the peripheral edge of the mounting table main body 31, and one end side of the first heat pipe 96a is located in the first temperature control flow path 97a. An annular second temperature control flow path 97b is formed at the lower end side peripheral portion of the mounting table main body 31, and one end side of the second heat pipe 96b is in the second temperature control flow path 97b. It is provided so that it may be located in.

  The first temperature control channel 97a and the second temperature control channel 97b are connected to each other as indicated by a dotted line in the drawing, for example, inside the mounting table body 31. The first temperature control channel 97 a extends downward on the periphery of the mounting table main body 31, extends outward from the apparatus main body 2, and is connected to the chiller unit 98. In the chiller unit 98, a temperature control medium such as Galden or Fluorinert is adjusted to a predetermined temperature, for example, 40 ° C. to 90 ° C. and supplied to the first temperature control flow path 97a. The temperature control medium supplied to the first temperature control flow path 97a flows from the first temperature control flow path 97a to the second temperature control flow path 97b, and from the second temperature control flow path 97b to the chiller unit. Return to 98.

  Thus, the mounting table main body 31 is provided with the first and second heat pipes 96a and 96b which are temperature adjusting sections, and one end side of the heat pipes 96a and 96b is a temperature control medium sent from the outside of the pressure vessel and Thus, heat is exchanged between the mounting table main body 31 and the outside of the pressure-resistant container, and the mounting table main body 31 acts as a temperature adjustment layer.

  In such a configuration, in the mounting table body 31, heat is transported by the first heat pipe 96 a and the second heat pipe 96 b so that the temperature of the mounting table body 31 becomes the same as the temperature of the temperature control medium. Done. As a result, the in-plane uniformity of the temperature of the mounting table main body 31 forming the bottom surface portion of the pressure vessel increases, so that the in-plane uniformity of heat radiation from the stage heater 88 toward the bottom surface portion of the pressure vessel can be further increased. The in-plane uniformity of the temperature of 88 can be further improved.

  Further, in the present invention, as shown in FIG. 15, when the support portion 88b of the stage heater 88 is long, the bottom portion of the pressure vessel (the portion where the support portion 88b of the mounting table main body 31 is provided) 1 is provided at the base of the portion extending downward of the mounting table main body 31 to provide a first temperature control flow path 99a that constitutes a temperature adjusting means made of Al or Cu. A temperature adjusting medium such as Galden or Fluorinert whose temperature is adjusted to a predetermined temperature may be passed through the adjusting flow path 99a. In this way, in the stage heater 88, the base part of the support part 88b is the part where heat is most easily dissipated, but the temperature of the base region of the part extending to the lower side of the mounting table body 31 close to this is controlled by the temperature control channel 99a. By doing so, it is possible to suppress an increase in temperature in the region, and to achieve in-plane uniformity of heat radiation from the stage heater 88 to the bottom surface of the pressure vessel.

  As shown in FIG. 15, when the supply path 85 is provided outside the mounting table main body 31, the second temperature forming the temperature adjusting means composed of Al or Cu is provided outside the supply path 85. By providing a temperature control channel 99b and passing a temperature control medium such as Galden or Fluorinert adjusted to a predetermined temperature through the temperature control channel 99b, and bringing the supply channel 85 into contact with the temperature control medium, The temperature of the supercritical fluid for heat insulation flowing through the supply path 85 may be adjusted. In this way, since the heat-insulating supercritical fluid whose temperature is adjusted with higher accuracy is passed through the flow path 91, the heat insulation efficiency between the stage heater 88 and the bottom surface of the pressure vessel is further improved. be able to. In this example, the first and second temperature control channels 99a and 99b are provided outside the pressure vessel, and pressure is not applied to them, so that the first and second temperature control channels 99a and 99b can be made of Al, Cu, or the like.

  Here, also in the examples shown in FIGS. 9 to 13 and 15, as in the example shown in FIG. 14, a heat pipe is embedded in the mounting table main body 31, and the mounting table main body 31 functions as a temperature adjustment layer. As shown in FIG. 1 and FIG. 7, a temperature adjustment layer is separately provided on the upper surface of the mounting table body 31, and the temperature adjustment flow path and heat pipe forming the temperature adjustment unit are embedded in the temperature adjustment layer to adjust the temperature. Heat may be transferred to the layer from the outside of the pressure vessel. Moreover, you may combine the example shown in FIG. 12, and the example shown in FIG. Also in the examples shown in FIGS. 11 to 15, for example, as shown in FIG. 10, the flow region of the processing fluid (supercritical fluid and source gas) and the flow region of the supercritical fluid for heat insulation are separated. You may make it provide.

  Furthermore, as described above, the stage heater 4 of the present invention may include a soaking plate 48 having a U-shaped cross section on a flat heater portion 47 made of SUS as shown in FIG. The soaking plate 48 is made of a material having a higher thermal conductivity than SUS, such as Al, Cu, AlN, SiC, or a composite material thereof. In this example, a recess 49 for dropping the wafer W is formed by the soaking plate 48, the thickness L5 of the heater portion 47 is, for example, about 10 mm, and the thickness L6 of the recess 49 portion of the soaking plate 48 is, for example, Each is formed to about 5 mm.

  As described above, since the pressure is uniformly applied to the planar stage heater, the strength of the heater itself can be small, and therefore, a material having a higher thermal conductivity than SUS can be used for the stage heater. At this time, a thermocouple (not shown) is embedded in, for example, the soaking plate 48. In such a stage heater, the concave portion 49 on which the wafer W is placed is made of a material having a thermal conductivity higher than that of SUS. Therefore, in this portion, heat is easily transferred in-plane, and the in-plane temperature is uniform. Sex can be secured. Furthermore, when the strength of the heater itself is not so high, the entire planar stage heater is made of a material having a higher thermal conductivity than SUS, for example, Al, Cu, AlN, SiC, or a composite material thereof. May be.

It is a schematic sectional drawing which shows an example of the high-pressure processing apparatus which concerns on this invention. It is a schematic perspective view which shows the stage heater which is a part of component of the high pressure processing apparatus which concerns on this invention, a heat insulation layer, and a temperature control layer. It is sectional drawing which shows the stage heater which is a part of component of the high pressure processing apparatus which concerns on this invention, a heat insulation layer, and a temperature control layer. It is an effect | action figure which shows a series of processes performed using the said high pressure processing apparatus. It is an effect | action figure which shows a series of processes performed using the said high pressure processing apparatus. It is a flowchart which shows a series of processes performed using the said high voltage | pressure processing apparatus. It is a schematic sectional drawing which shows the other example of the high voltage | pressure processing apparatus which concerns on this invention. It is a schematic sectional drawing which shows the other example of the high-pressure processing apparatus which concerns on this invention. It is a schematic sectional drawing which shows the other example of the high-pressure processing apparatus which concerns on this invention. It is a schematic sectional drawing which shows the other example of the high-pressure processing apparatus which concerns on this invention. It is a schematic sectional drawing which shows the other example of the high-pressure processing apparatus which concerns on this invention. It is a schematic sectional drawing which shows the other example of the high-pressure processing apparatus which concerns on this invention. It is a schematic sectional drawing which shows the other example of the high-pressure processing apparatus which concerns on this invention. It is a schematic sectional drawing which shows the other example of the high-pressure processing apparatus which concerns on this invention. It is a schematic sectional drawing which shows the other example of the high-pressure processing apparatus which concerns on this invention. It is a schematic sectional drawing which shows the other example of the high-pressure processing apparatus which concerns on this invention. It is explanatory drawing which shows the conventional high-pressure processing apparatus. It is a characteristic view which shows the relationship between the film thickness of Cu film formed on the surface of a wafer, and the temperature of a stage heater. It is a characteristic view which shows the relationship between the temperature of a stage heater, the position on a wafer, and the film thickness of Cu film formed on the surface of a wafer.

Explanation of symbols

F Deposition processing space W Semiconductor wafer 2 Device main body 20 Pressure-resistant frame member 21 Upper lid 3 Mounting base 31 Mounting base main body 4 Stage heater 41 Recess 42 Sheath heater 43 Thermocouple 51 Thermal insulation layer 53 Temperature adjustment layer 55 Temperature control channel 71 Heat pipe 84 Insulating supercritical fluid flow path 85 Insulating supercritical fluid supply path 100 Raw material mixing / heating device 101 Precursor supply unit 110 Reducing agent mixing / heating device 111 Reducing agent supply unit 120 Medium storage tank

Claims (11)

In a high-pressure processing apparatus for forming a film on a substrate by supplying a processing fluid containing a supercritical fluid and a film-forming raw material into a pressure-resistant container,
A stage heater on which the substrate is placed and provided with a heating element;
A heat insulating layer provided on the lower side of the stage heater and having a thermal conductivity smaller than the thermal conductivity of the material of the pressure vessel;
A temperature adjustment layer provided between the heat insulation layer and the bottom portion of the pressure vessel, and provided with a temperature adjustment portion for transferring heat to and from the outside of the pressure vessel. High pressure processing equipment characterized by.   The high-pressure processing apparatus according to claim 1, wherein the temperature adjustment unit is a flow path through which a temperature adjustment medium flows.   The high-pressure processing apparatus according to claim 1, wherein the temperature adjusting unit is a heat pipe having one end located in a flow path of a temperature control medium sent from the outside of the pressure vessel.   4. The temperature control layer according to claim 1, wherein the temperature adjustment layer forms a part of the bottom surface portion of the pressure vessel, instead of being interposed between the heat insulating layer and the bottom surface portion of the pressure vessel. The high-pressure processing apparatus according to claim 1. In a high-pressure processing apparatus for forming a film on a substrate by supplying a processing fluid containing a supercritical fluid and a film-forming raw material into a pressure-resistant container,
A stage heater on which the substrate is placed and provided with a heating element;
A high-pressure processing apparatus comprising: a passage for passing a supercritical fluid for heat insulation provided between the stage heater and the bottom surface of the pressure vessel.   A temperature adjustment layer provided with a temperature adjustment portion for transferring heat to and from the outside of the pressure vessel so as to be interposed between the flow path of the supercritical fluid and the bottom portion of the pressure vessel. The high-pressure processing apparatus according to claim 5.   The high-pressure processing apparatus according to claim 6, wherein the temperature adjustment unit is a flow path through which a temperature adjustment medium flows.   The high-pressure processing apparatus according to claim 6, wherein the temperature adjusting unit is a heat pipe having one end located in a flow path of a temperature control medium sent from the outside of the pressure vessel.   The stage heater includes a planar heater portion in which a heating unit is embedded, and a support portion extending downward from a substantially central portion of the heater portion, and the portion of the support portion in contact with the heater portion includes: The high-pressure processing apparatus according to any one of claims 5 to 8, wherein a heat insulating layer having a thermal conductivity smaller than that of the material of the pressure vessel is provided.   The stage heater includes a planar heater portion in which a heating means is embedded, and a support portion extending downward from a substantially central portion of the heater portion, and a part of the bottom portion of the pressure vessel is the supercritical The heat insulating layer having a thermal conductivity smaller than the thermal conductivity of the material of the pressure vessel is provided at a portion in contact with the fluid flow path. High pressure processing equipment.   11. The high-pressure processing apparatus according to claim 5, further comprising a temperature adjusting unit configured to adjust a temperature of the supercritical fluid supplied to the flow path of the supercritical fluid.

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