Thin film deposition apparatus and control method for the thin film deposition apparatus

Abstract

The present invention provides a film deposition apparatus capable of adjusting purity and quality, and a control method for the film deposition apparatus. [Solution] The regeneration mechanism 600 comprises a chamber 100 for containing metal particles, a raw material gas storage unit 200 connected to the chamber 100 for storing raw material gas 200A for forming a film on the metal particles, a reaction gas storage unit 300 connected to the chamber 100 for storing reaction gas 300A for reacting with the raw material gas 200A, a tank for containing the exhausted raw material gas 200A, a cooling unit for cooling the raw material gas 200A and collecting the raw material, a heating unit for sublimating the raw material to generate regenerated raw material gas, and a collection amount detection sensor for detecting the amount of raw material collected, a suction pump 500 for adjusting the pressure of the tank, and a return supply path 230 for supplying regenerated raw material gas from the regeneration mechanism 600 to the chamber 100.

Description

Technical Field

[0001] The present invention relates to a film forming apparatus and a method for controlling the film forming apparatus.

Background Art

[0002] Patent Document 1 discloses a configuration of an atomic layer deposition film forming apparatus in which a source gas (also referred to as virgin gas) is supplied into a reaction chamber, adsorbed on the surface of a substrate by only one atomic layer of the source gas, and then reacted with a subsequent reaction gas to form a film on the surface of the substrate. Since the source gas is adsorbed on the substrate by only one atomic layer, the surplus that is not used is discarded, resulting in a problem of increased source gas cost. Therefore, by using a collecting means for collecting the source contained in the discharged source gas, the regenerated source gas (also referred to as recycled gas) can be reused.

Prior Art Documents

Patent Documents

[0003]

Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0004] However, the configuration described in Patent Document 1 has a problem that it is difficult to control the purity and quality of the regenerated source gas. In other words, depending on the use of the film to be formed, it is required to adjust the supply amount of the regenerated source gas with respect to the source gas.

Means for Solving the Problems

[0005] The film deposition apparatus comprises a chamber for housing a film deposition material, a raw material gas storage unit connected to the chamber for storing raw material gas for deposition on the film deposition material, a reaction gas storage unit connected to the chamber for storing reaction gas for reaction with the raw material gas, a tank for housing the exhausted raw material gas, a cooling unit for cooling the raw material gas and collecting raw materials, a heating unit for sublimating the raw materials to generate regenerated raw material gas, a collection amount detection sensor for detecting the amount of collected raw materials, a suction pump for adjusting the pressure of the tank, and a return supply path for supplying the regenerated raw material gas from the regeneration mechanism to the chamber.

[0006] The control method for the film deposition apparatus comprises: a chamber for housing a member to be film-deposited; a raw material gas storage unit for storing raw material gas for film deposition on the member to be film-deposited; a first valve for switching the supply of the raw material gas to the chamber or the supply of recycled raw material gas for reusing the raw material gas; a reaction gas storage unit for storing reaction gas for reacting with the raw material gas; a second valve for controlling the supply of the reaction gas to the chamber; a raw material gas exhaust path connected to the chamber and for exhausting the raw material gas from the chamber via a third valve; a reaction gas exhaust path connected to the chamber and for exhausting the reaction gas from the chamber via a fourth valve; a suction pump for exhausting at least one of the raw material gas and the reaction gas from the chamber; a cooling unit provided in the raw material gas exhaust path for collecting raw materials contained in the raw material gas by cooling; and a heating unit for generating recycled raw material gas by sublimating the raw materials by heating. A control method for a film deposition apparatus comprising: a regeneration mechanism having; a fifth valve provided between the regeneration mechanism and the suction pump in the raw material gas exhaust path, which is open when the raw material gas is exhausted; and a return supply path connected between the regeneration mechanism and the first valve, which returns the regenerated raw material gas to the chamber via a sixth valve, wherein the process of supplying the raw material gas to the chamber and exhausting the raw material gas from the chamber, supplying the reaction gas to the chamber and exhausting the reaction gas from the chamber is repeated, wherein when the raw material gas is exhausted, the sixth valve is closed and the cooling unit is turned on; when the raw material collected in the cooling unit reaches a predetermined amount, the heating unit is turned on; and when the regenerated raw material gas is supplied from the regeneration mechanism to the chamber via the return supply path, the third valve and the fifth valve are closed and the sixth valve is open. [Brief explanation of the drawing]

[0007] [Figure 1] A schematic diagram showing the configuration of the film deposition apparatus. [Figure 2] A cross-sectional view showing the structure of particles with an insulating film. [Figure 3] A cross-sectional view showing the configuration of the regeneration mechanism. [Figure 4] A flowchart illustrating the film deposition method. [Figure 5] A diagram showing some of the steps in the film deposition method. [Figure 6] A flowchart illustrating the pressure adjustment method used in the film deposition process. [Figure 7] A diagram illustrating the method for detecting the amount of raw material collected. [Figure 8] A diagram illustrating the method for detecting the amount of raw material collected. [Modes for carrying out the invention]

[0008] The film deposition apparatus 1000 and the film deposition method will be described below with reference to the drawings. First, the configuration of the film deposition apparatus 1000 will be described with reference to Figure 1.

[0009] As shown in Figure 1, the film deposition apparatus 1000 is an apparatus that deposits an insulating film 32 on the surface of metal particles 31, which are to be treated, by atomic layer deposition (ALD), for example, to form insulating film-coated particles 33 (see Figure 2).

[0010] The film deposition apparatus 1000 includes a chamber 100, a raw material gas storage section 200, a reaction gas storage section 300, a plurality of valves 410 to 460, a raw material gas supply path 210, a raw material gas exhaust path 220, a reaction gas supply path 310, a reaction gas exhaust path 320, a suction pump 500, a regeneration mechanism 600, and a return supply path 230.

[0011] Chamber 100 is rigid and airtight, and has a volume of, for example, 10 L to 100 L. Chamber 100 has an opening / closing section (not shown), through which trays (not shown) holding metal particles 31 are loaded into and unloaded from Chamber 100. With the metal particles 31 contained inside Chamber 100, an insulating film 32 is formed on the surface of the metal particles 31.

[0012] Chamber 100 maintains a reduced pressure state by exhausting its interior. Examples of materials used to construct chamber 100 include glass materials such as quartz glass, ceramic materials such as alumina, and metallic materials such as stainless steel, aluminum, and titanium.

[0013] Chamber 100 is connected to a raw material gas storage unit 200 and a reaction gas storage unit 300. The raw material gas storage unit 200 stores raw material gas 200A for supply to Chamber 100. A raw material gas supply route 210, which is a pipe, is connected between the raw material gas storage unit 200 and Chamber 100.

[0014] The raw material gas supply path 210 is equipped with a first main valve 411 and a first sub-valve 412. The first main valve 411 controls the supply from the raw material gas storage section 200 to the chamber 100. The first sub-valve 412 controls the supply of regenerated raw material gas 200C to the chamber 100 via the return supply path 230, which is a pipe.

[0015] The first valve 410 has a first main valve 411 and a first sub-valve 412. By switching between the first main valve 411 and the first sub-valve 412, it is possible to select whether to supply raw material gas 200A from the raw material gas storage unit 200 or to supply regenerated raw material gas 200C from the regeneration mechanism 600 into the chamber 100.

[0016] When the raw material gas 200A in the chamber 100 is exhausted via the raw material gas exhaust path 220, which is a pipe, the first sub-valve 412 is closed. In this way, since the first sub-valve 412 is closed when the raw material gas 200A is exhausted, it is possible to prevent the generated regenerated raw material gas 200C from flowing into the chamber 100. Therefore, it is possible to prevent the mixing of raw material gas 200A and regenerated raw material gas 200C.

[0017] As the raw material gas 200A, for example, a gas containing a precursor of the insulating film 32 can be mentioned. Specifically, for example, when forming the silicon-based insulating film 32, as the raw material gas 200A, secondary amines such as dimethylamine, methylethylamine, and diethylamine, and reactants of secondary amines and trihalosilanes such as tris(dimethylamino)silane, bis(diethylamino)silane, and bis(tert-butylamino)silane can be mentioned.

[0018] In the reaction gas storage section 300, the reaction gas 300A for supplying into the chamber 100 is stored. Between the reaction gas storage section 300 and the chamber 100, a reaction gas supply path 310 which is a pipe is connected. In the reaction gas supply path 310, a second valve 420 is provided. By opening and closing the second valve 420, the reaction gas 300A necessary for forming the insulating film 32 can be supplied into the chamber 100, and the partial pressure of the reaction gas 300A in the chamber 100 can be adjusted.

[0019] The reaction gas 300A is, for example, an oxidizing agent such as oxygen gas. As the oxidizing agent, for example, ozone, plasma oxygen, water vapor, etc. can be mentioned. By using ozone as the oxidizing agent, a more dense and uniform-thickness insulating film 32 can be formed more efficiently.

[0020] The raw material gas 200A and the reaction gas 300A are supplied together with a carrier gas 250A mainly composed of an inert gas such as nitrogen gas or argon gas as necessary. The raw material gas storage section 200 is connected to the carrier gas storage section 250 via a pipe 251. In the pipe 251, a valve 252 and a flow controller 253 are provided.

[0021] The chamber 100 has a plasma generation section (not shown) that generates oxygen plasma using oxygen gas. Thus, since the plasma generation section is arranged in the chamber 100, an insulating film 32 can be formed on the surface of the metal particles 31 by utilizing the chemical reaction between the raw material gas 200A and the reaction gas 300A.

[0022] The suction pump 500 is, for example, a vacuum pump. The suction pump 500 exhausts the raw material gas 200A and reaction gas 300A supplied to the chamber 100 and the regeneration mechanism 600. Between the chamber 100 and the suction pump 500 are raw material gas exhaust paths 220 and 221, which are pipes for exhausting the raw material gas 200A, and a reaction gas exhaust path 320, which is a pipe for exhausting the reaction gas 300A.

[0023] A regeneration mechanism 600 is connected between the raw material gas exhaust path 220 and the raw material gas exhaust path 221. The regeneration mechanism 600 includes a cooling section 610 (see Figure 3) that collects raw material 200B contained in the raw material gas 200A by cooling, and a heating section 620 that generates regenerated raw material gas 200C by sublimating the raw material 200B by heating.

[0024] A third valve 430 is provided in the raw material gas exhaust path 220. A fifth valve 450 is provided in the raw material gas exhaust path 221. By opening and closing the third valve 430 and the fifth valve 450, raw material gas 200A can be supplied to the regeneration mechanism 600, or raw material gas 200A can be exhausted from the regeneration mechanism 600.

[0025] A fourth valve 440 is provided in the reaction gas exhaust path 320. By opening and closing the fourth valve 440, the reaction gas 300A in the chamber 100 can be exhausted, and the pressure inside the chamber 100 can be reduced. The pressure inside the chamber 100 is measured by a pressure gauge 110.

[0026] A return supply path 230 is connected between the regeneration mechanism 600 and the chamber 100, specifically between the regeneration mechanism 600 and the first sub-valve 412. A sixth valve 460 is provided in the return supply path 230. By opening and closing the sixth valve 460, the regenerated raw material gas 200C generated in the regeneration mechanism 600 can be supplied to the chamber 100.

[0027] Furthermore, the regeneration mechanism 600 is connected via piping 261 to a carrier gas storage section 260, which stores the carrier gas 260A used when supplying the regeneration raw material gas 200C from the regeneration mechanism 600 to the chamber 100. A valve 262 and a flow controller 263 are provided in the piping 261.

[0028] Next, the structure of the insulating film-coated particle 33 will be described with reference to Figure 2.

[0029] As shown in Figure 2, the insulating film-coated particle 33 comprises a metal particle 31 and an insulating film 32 formed on the surface of the metal particle 31.

[0030] Examples of materials that make up the metal particles 31 include soft magnetic metal materials. When metal particles 31 made of soft magnetic metal materials are used in magnetic elements such as inductors, it is necessary to ensure insulation between the metal particles 31.

[0031] By using the film deposition apparatus 1000 described above, an insulating film 32 with a sufficiently thin film thickness and high coverage can be formed. This results in insulating film-coated particles 33 that can enhance the magnetic and insulating properties of magnetic elements. Furthermore, because the insulating film 32 formed by atomic layer deposition is dense, it also contributes to the realization of insulating film-coated particles 33 with high insulating properties.

[0032] Examples of soft magnetic metal materials include pure iron, Fe-Si alloys such as silicon steel, Fe-Ni alloys such as permalloy, Fe-Co alloys such as permendur, Fe-Si-Al alloys such as sendust, Fe-Cr-Si alloys and various other Fe-based alloys, as well as various Ni-based alloys, various Co-based alloys, and various amorphous alloys. Among these, examples of amorphous alloys include Fe-based alloys such as Fe-Si-B, Fe-Si-BC, Fe-Si-B-Cr-C, Fe-Si-Cr, Fe-B, Fe-PC, Fe-Co-Si-B, Fe-Si-B-Nb, and Fe-Zr-B, Ni-based alloys such as Ni-Si-B and Ni-PB, and Co-based alloys such as Co-Si-B.

[0033] The average particle size of the metal particles 31 is, for example, 2 μm or less. However, the average particle size of the metal particles 31 is not limited to 2 μm or less, and may be, for example, between 0.1 μm and 50.0 μm.

[0034] Examples of constituent materials for the insulating film 32 include 3DMAS (tris(dimethylamino)silane), TMA (trimethylaluminum), and TBTMT (tert-butylimidotris(ethylmethylamino)tantalum). However, the materials are not limited to these, and oxides such as silicon dioxide, hafnium oxide, tantalum oxide, titanium dioxide, and chromium oxide may also be used.

[0035] Next, the configuration of the regeneration mechanism 600 will be described with reference to Figure 3.

[0036] As shown in Figure 3, the regeneration mechanism 600 comprises a tank 601, a plurality of cooling units 610 arranged around the tank, a plurality of heating units 620 arranged alternately with the cooling units 610, and collection amount detection sensors 640 and 650 for detecting the amount of raw material 200B collected. The regeneration mechanism 600 is also called, for example, a cold trap. The collection amount detection sensors 640 and 650 will be described with reference to Figures 7 and 8.

[0037] Tank 601 is connected to a raw material gas exhaust path 220, piping 261, another raw material gas exhaust path 221, and a return supply path 230. A pressure gauge 630 is also installed in tank 601.

[0038] For the cooling section 610, for example, a refrigerant such as a Peltier element or water cooling is used. For the heating section 620, for example, a heating element such as a ribbon heater or silicone rubber is used.

[0039] As shown in Figures 1 and 3, when collecting the raw material gas 200A exhausted from the chamber 100, the cooling unit 610 of the regeneration mechanism 600 is turned ON, the third valve 430 and the fifth valve 450 are opened, and the first main valve 411 and the first sub-valve 412 are closed. At this time, the supply of regenerated raw material gas 200C from the return supply path 230 to the chamber 100 is shut off.

[0040] The raw material gas 200A exhausted from the chamber 100 is supplied to the regeneration mechanism 600 via the raw material gas exhaust path 220. The supplied raw material gas 200A is cooled by a plurality of cooling units 610 arranged around the tank 601.

[0041] When the gaseous raw material gas 200A is cooled, it liquefies, or in other words, solidifies, into the tank 601 as raw material 200B (see Figure 5). The raw material gas 200A containing impurities that were not liquefied is exhausted to the suction pump 500 through the raw material gas exhaust path 221.

[0042] As shown in Figures 1 and 3, when reusing the recycled raw material gas 200C using the regeneration mechanism 600, the third valve 430, the fifth valve 450, and the sixth valve 460 are closed, and the heating unit 620 of the regeneration mechanism 600 is turned ON.

[0043] While controlling the temperature and pressure inside the tank 601 of the regeneration mechanism 600, the raw material 200B stored in the tank 601 is heated by the heating unit 620, causing the raw material 200B to sublimate and be generated as regenerated raw material gas 200C.

[0044] The recycled raw material gas 200C is supplied to the chamber 100 via piping 261, together with a carrier gas mainly composed of inert gases such as nitrogen gas and argon gas supplied from the carrier gas storage unit 260. At this time, the optimal supply amount and rate of the recycled raw material gas 200C are adjusted using a flow controller 263 provided in piping 261.

[0045] Thus, when the raw material gas 200A is exhausted from the chamber 100, the cooling unit 610 is turned on, allowing the raw material 200B contained in the raw material gas 200A to be collected by the cooling unit 610. On the other hand, when the reaction gas 300A is exhausted from the chamber 100, the heating unit 620 is turned on, allowing the raw material 200B collected by the cooling unit 610 to be sublimated to generate recycled raw material gas 200C. Therefore, it becomes possible to reuse the raw material gas 200A that was previously discarded, thereby reducing raw material costs.

[0046] Furthermore, while the reaction gas 300A is being exhausted, specifically while the reaction gas 300A is being supplied to the chamber 100, while the raw material gas 200A and the reaction gas 300A are reacting in the chamber 100, and while the reaction gas 300A is being exhausted from the chamber 100, the regeneration mechanism 600 generates regenerated raw material gas 200C from the raw material 200B, thus shortening the cycle time.

[0047] Next, a film deposition method for forming an insulating film 32 on the surface of metal particles 31 and a control method for the film deposition apparatus 1000 will be described with reference to Figures 1, 4, 5, and 6. The method used for depositing the insulating film 32 is atomic layer deposition.

[0048] Furthermore, the control method for the film deposition apparatus 1000 involves repeatedly supplying raw material gas 200A to the chamber 100 and exhausting the raw material gas 200A from the chamber 100, supplying reaction gas 300A to the chamber 100, and exhausting the reaction gas 300A from the chamber 100.

[0049] As shown in Figure 4, in step S11, the metal particles 31 are placed inside the chamber 100. Specifically, for example, an opening / closing part (not shown) of the chamber 100 is opened and a tray on which the metal particles 31 are arranged is placed inside.

[0050] Next, in step S12, raw material gas 200A is supplied into the chamber 100. Specifically, raw material gas 200A is supplied from the raw material gas storage unit 200 to the chamber 100 via the raw material gas supply path 210. The first main valve 411 and the first sub-valve 412 are in the open state. The second valve 420 is in the closed state.

[0051] The temperature of the raw material gas storage section 200 is, for example, 25°C to 60°C. The temperature of the raw material gas supply path 210 is, for example, 80°C to 150°C. The flow rate of the raw material gas 200A is, for example, 10 sccm to 100 sccm. The temperature of the chamber 100 is, for example, 200°C to 300°C.

[0052] The introduced raw material gas 200A is adsorbed onto the surface of the metal particles 31. At this time, once the raw material gas 200A is adsorbed onto the surface of the metal particles 31, it is difficult for it to adsorb in any further layers. Therefore, it is possible to control the thickness of the final insulating film 32 with high precision. In addition, since the raw material gas 200A also wraps around and adsorbs into the shadows and gaps of the metal particles 31, the thickness of the insulating film 32 is made uniform.

[0053] In the case of sealed film deposition, the third valve 430 and the fourth valve 440 are in the closed state. On the other hand, in the case of flow deposition, the third valve 430 is in the open state and the fourth valve 440 is in the closed state.

[0054] Next, in step S13, the raw material gas 200A is exhausted. Specifically, the suction pump 500 is used to exhaust the excess raw material gas 200A used for film formation from the chamber 100 through the raw material gas exhaust path 220 and the regeneration mechanism 600.

[0055] The third valve 430 and the fifth valve 450 are in the open state. The first sub-valve 412, the fourth valve 440 located in the reaction gas exhaust path 320, and the sixth valve 460 located in the return supply path 230 are in the closed state. The cooling unit 610 of the regeneration mechanism 600 is in the ON state. The raw material gas supply process and the raw material gas exhaust process may have at least some overlapping time.

[0056] Next, in step S14, raw material 200B is cold-trapped from raw material gas 200A. Specifically, the temperature of the cooling unit 610 is, for example, 15°C to 25°C. When the gaseous raw material gas 200A is cooled, it is liquefied, or in other words, solidified, into tank 601 as raw material 200B (see Figure 5). By-products that were not liquefied are exhausted to the suction pump 500 through the raw material gas exhaust path 221.

[0057] Next, in step S15, reaction gas 300A is supplied into the chamber 100. Specifically, the second valve 420 provided in the reaction gas supply path 310 is opened to supply reaction gas 300A from the reaction gas storage section 300 into the chamber 100. The first sub-valve 412 is closed.

[0058] In the case of sealed film deposition, the third valve 430 and the fourth valve 440 are in the closed state. On the other hand, in the case of flow deposition, the third valve 430 is in the closed state and the fourth valve 440 is in the open state.

[0059] As mentioned above, the reaction gas 300A can be an oxidizing agent such as ozone, plasma oxygen, or water vapor. The reaction gas 300A reacts with the raw material gas 200A adsorbed on the surface of the metal particles 31 to form an insulating film 32.

[0060] The temperature of the reaction gas storage section 300 is, for example, 25°C to 60°C. The temperature of the reaction gas supply path 310 is, for example, 80°C to 150°C. The temperature of the chamber 100 is, for example, 200°C to 300°C.

[0061] Next, in step S16, the reaction gas 300A is exhausted. Specifically, the fourth valve 440, located in the reaction gas exhaust path 320, is opened to exhaust the reaction gas 300A from the chamber 100. The third valve 430 and the fifth valve 450 remain closed. The temperature of the reaction gas exhaust path 320 is, for example, 100°C to 200°C. Note that there may be at least some overlap between the reaction gas supply process and the reaction gas exhaust process.

[0062] Next, in step S17, the regenerated raw material gas 200C is generated. Specifically, when the raw material 200B collected in the cooling section 610 of the regeneration mechanism 600 reaches a predetermined amount, the heating section 620 is turned on. The collection of raw material 200B in the cooling section 610 is carried out in steps S14 to S16 described above.

[0063] When generating the recycled raw material gas 200C, the third valve 430 provided in the raw material gas exhaust path 220 is closed. The heating section 620 of the regeneration mechanism 600 is heated to heat the collected raw material 200B and adjust its pressure. Pressure adjustment is performed, for example, using a suction pump 500. In this way, the recycled raw material gas 200C is generated by the sublimation and re-vaporization of the raw material 200B. The temperature of the heating section 620 is, for example, 25°C to 60°C.

[0064] Next, in step S18, the regenerated raw material gas 200C is supplied into the chamber 100. Specifically, the sixth valve 460 and the first sub-valve 412, which are located in the return supply path 230, are opened, and the regenerated raw material gas 200C generated in the regeneration mechanism 600 is supplied into the chamber 100. The temperature of the return supply path 230 is, for example, 80°C to 150°C.

[0065] The third valve 430, the fifth valve 450, and valve 264 are in the closed position. If the pressure inside the regeneration mechanism 600 does not reach the specified value, as shown in Figure 5, valve 264 may be opened and carrier gas 260A, mainly composed of inert gases such as nitrogen gas or argon gas, may be supplied from the carrier gas storage section 260 to the regeneration mechanism 600 to adjust the pressure inside the regeneration mechanism 600.

[0066] Parameters of the regeneration mechanism 600 include, for example, the temperature of tank 601, the pressure of tank 601, the flow rate of carrier gas 260A, and the pressure of carrier gas 260A. According to this, even if the molecular weight of the raw material 200B is large due to its characteristics and simple gasification alone is difficult, the regenerated raw material gas 200C can be sent to the return supply path 230 by utilizing carrier gas 260A.

[0067] Next, an example of a method for adjusting the pressure of the regeneration mechanism 600 will be explained with reference to Figure 6.

[0068] As shown in Figure 6, in step S21, the tank 601 is heated. In step S22, it is determined whether the pressure in the tank 601 is sufficient. If it is sufficient, the process proceeds to step S23, and the supply of recycled raw material gas 200C is started.

[0069] If it is determined in step S22 that the pressure in tank 601 is insufficient, the process proceeds to step S24. In step S24, it is determined whether the pressure in tank 601, in other words, the recycled raw material gas 200C, is controllable. If it is controllable, the process proceeds to step S25 to adjust the temperature of tank 601, and then proceeds to step S21. If it is determined in step S24 that the pressure is not controllable, the process is terminated.

[0070] As an example, the pressure adjustment method when using 3DMAS as raw material 200B will be explained. The temperature of tank 601 is, for example, 40°C. The pressure of tank 601 is, for example, 1300 Pa. The flow rate of carrier gas 260A is, for example, 50 sccm. The pressure of carrier gas 260A is, for example, 0.2 MPa.

[0071] Furthermore, depending on the required thickness of the insulating film 32, the supply and exhaust of the raw material gas 200A and the supply and exhaust of the reaction gas 300A can be repeated. The thickness of the insulating film 32 can be increased according to the number of repetitions. This makes it easy to obtain the desired thickness.

[0072] Subsequently, the insulating film-coated particles 33 may be subjected to post-treatment as needed. Examples of post-treatment include static elimination treatment and radical treatment. Of these, static elimination treatment is a treatment that reduces the amount of charge due to the charging of the insulating film-coated particles 33. For example, an ionizer can be used for static elimination treatment.

[0073] Examples of constituent materials for the formed insulating film 32 include oxides such as silicon oxide, hafnium oxide, tantalum oxide, titanium oxide, and chromium oxide, and nitrides such as aluminum nitride, titanium nitride, and tantalum nitride. The thickness of the insulating film 32 is not particularly limited, but as an example, it is between 1 nm and 500 nm.

[0074] Next, with reference to Figures 7 and 8, the liquid volume of raw material 200B, which becomes the recycled raw material gas 200C, i.e., the method for detecting the amount collected, and the method of use will be explained. Figure 7 shows the method for detecting the amount of raw material 200B collected when an ultrasonic liquid level gauge is used as the collection amount detection sensor 640. Figure 8 shows the method for detecting the amount of raw material 200B collected when a weighing scale is used as the collection amount detection sensor 650.

[0075] As shown in Figure 7, when using the collection amount detection sensor 640, the method for detecting the amount of raw material 200B collected requires that the tank 601 be sealed and that the collection amount detection sensor 640 be installed in a manner that matches the characteristics of the raw material 200B. The reason for making the tank sealable is to prevent leakage of liquid or gas.

[0076] For example, when using 3DMAS as the raw material 200B, it is preferable to use the collection amount detection sensor 640 described above. Although capacitive and float type sensors are available, when using an ALD device, it is preferable to use an ultrasonic collection amount detection sensor 640, considering safety and detection capability.

[0077] As shown in Figure 8, when using the collection amount detection sensor 650, an electronic balance capable of detecting the volume by weight including the tank 601 can be used to detect the amount of raw material 200B collected. When detecting the amount of collected material, it is preferable to use spiral pipes 261a, 220a, 221a, and 230 in the middle of the piping so as not to affect the weight of the tank 601.

[0078] In this way, by detecting the amount of raw material 200B collected, the heating unit 620 can be turned on when the collected amount reaches a predetermined level. The method for determining the predetermined amount can be determined in advance by calculating the number of cycles required for film formation based on the algorithm's calculations.

[0079] Next, we will explain how to use recycled raw material gas 200C using the collection amount detection method described above. First, we will explain how to use raw material gas 200A and recycled raw material gas 200C.

[0080] First, the raw material gas 200A is exhausted and cold-trapped in the regeneration mechanism 600. This collects the raw material 200B. Next, the amount of collected raw material 200B is continuously monitored using the detection method described above. After this, while the insulating film 32 is being formed by reacting the raw material gas 200A and reaction gas 300A in the chamber 100, the regeneration mechanism 600 is heated to start vaporizing the raw material 200B. Next, the cycle for starting the use of the regenerated raw material gas 200C is calculated according to the number of film formation processes. From the cycle for supplying the regenerated raw material gas 200C, the first main valve 411, the first sub-valve 412, and the sixth valve 460 are opened, and the raw material gas 200A and the regenerated raw material gas 200C are supplied into the chamber 100.

[0081] Next, we will explain how to use the system when only recycled raw material gas 200C is used.

[0082] First, the amount of raw material 200B collected in the cold trap in the regeneration mechanism 600, i.e., the processing cycle is calculated according to the amount collected. Next, while the raw material gas 200A and reaction gas 300A are reacted in the chamber 100 to form an insulating film 32, the regeneration mechanism 600 is heated to start vaporizing the raw material 200B. Subsequently, from the cycle in which the regenerated raw material gas 200C is supplied, the first main valve 411, the first sub-valve 412, and the sixth valve 460 are opened, and the regenerated raw material gas 200C is supplied into the chamber 100.

[0083] Thus, since the regeneration mechanism 600 has collection amount detection sensors 640 and 650, it is possible to detect the amount of raw material 200B collected in the cooling unit 610, and the amount of regenerated raw material gas 200C to be supplied can be determined based on the collection amount. Therefore, it is possible to adjust the supply amount of regenerated raw material gas 200C relative to the supply amount of raw material gas 200A, and the purity and quality of the raw material gas 200A can be controlled. In addition, for example, the supply amount of regenerated raw material gas 200C can be adjusted based on the application of the film to be formed.

[0084] Next, we will explain the selection of the gas mode used for film deposition.

[0085] Three gas modes are possible: using only raw material gas 200A, using only recycled raw material gas 200C, and using a mixture of raw material gas 200A and recycled raw material gas 200C.

[0086] When using only 200A as the raw material gas, the purity and quality of the resulting film are high. Therefore, even if the cost of using 200A as the raw material gas is high, it can be used for applications where, for example, insulating properties are required for insulating films, or conductive properties are required for conductive films.

[0087] When using only recycled raw material gas 200C, the purity and quality of the resulting film are low. Therefore, it can be used for applications where, for example, an insulating film only needs to provide a superficial covering, or a conductive film only needs to conduct electricity.

[0088] When using a mixed gas of raw material gas 200A and recycled raw material gas 200C, the purity and quality of the deposited film are intermediate between those of the gases mentioned above. When using a mixed gas, it is desirable to change the ratio of raw material gas 200A to recycled raw material gas 200C depending on the purpose of the film being deposited. Increasing the use of recycled raw material gas 200C can reduce the cost of film deposition.

[0089] Furthermore, regarding the method of selecting the mode of the gas to be used, it is preferable, for example, to perform a compositional analysis in advance and select the mode based on the results. With this method, the cooling section 610 and the heating section 620 of the regeneration mechanism 600 can be switched according to the mode, thereby improving the cooling efficiency in collection and the heating efficiency in sublimation. In addition, the regeneration mechanism 600 can be made to function more efficiently.

[0090] As described above, the film deposition apparatus 1000 of this embodiment includes a chamber 100 for containing metal particles 31, a raw material gas storage unit 200 connected to the chamber 100 for storing raw material gas 200A for forming a film on the metal particles 31, a reaction gas storage unit 300 connected to the chamber 100 for storing reaction gas 300A for reacting with the raw material gas 200A, a tank 601 for containing the exhausted raw material gas 200A, a regeneration mechanism 600 having a cooling unit 610 for collecting raw material 200B from the raw material gas 200A, a heating unit 620 for generating regenerated raw material gas 200C by sublimating the raw material 200B, and collection amount detection sensors 640, 650 for detecting the amount of raw material 200B collected, a suction pump 500 for adjusting the pressure of the tank 601, and a return supply path 230 for supplying regenerated raw material gas 200C from the regeneration mechanism 600 to the chamber 100.

[0091] With this configuration, since the regeneration mechanism 600 has collection amount detection sensors 640 and 650, it is possible to detect the amount of raw material 200B collected in the cooling unit 610, and the amount of regenerated raw material gas 200C to be supplied can be determined based on the collection amount. Therefore, it is possible to adjust the supply amount of regenerated raw material gas 200C relative to the supply amount of raw material gas 200A, and the purity and quality of the raw material gas 200A can be controlled. In addition, for example, the supply amount of regenerated raw material gas 200C can be adjusted based on the application of the film to be formed.

[0092] Furthermore, the control method of the film deposition apparatus 1000 in this embodiment includes a chamber 100 for containing metal particles 31, a raw material gas storage unit 200 for storing raw material gas 200A for forming a film on the metal particles 31, a first valve 410 for switching the supply of raw material gas 200A to the chamber 100 or the supply of recycled raw material gas 200C for reusing raw material gas 200A, a reaction gas storage unit 300 for storing reaction gas 300A for reacting with the raw material gas 200A, a second valve 420 for controlling the supply of reaction gas 300A to the chamber 100, and connected to the chamber 100. A raw material gas exhaust path 220 for exhausting the raw material gas 200A from the chamber 100 via a third valve 430; a reaction gas exhaust path 320 connected to the chamber 100 for exhausting the reaction gas 300A from the chamber 100 via a fourth valve 440; a suction pump 500 for exhausting at least one of the raw material gas 200A and the reaction gas 300A from the chamber 100; a cooling unit 610 provided in the raw material gas exhaust path 220 for collecting raw material 200B contained in the raw material gas 200A by cooling; and a regenerating raw material by sublimating the raw material 200B by heating. The system includes a regeneration mechanism 600 having a heating unit 620 for generating gas 200C, a fifth valve 450 provided between the regeneration mechanism 600 and the suction pump 500 in the raw material gas exhaust path 220 which is open when raw material gas 200A is exhausted, and a return supply path 230 connected between the regeneration mechanism 600 and the first valve 410 which returns and supplies regenerated raw material gas 200C to the chamber 100 via a sixth valve 460, and is used for supplying raw material gas 200A to the chamber 100, exhausting raw material gas 200A from the chamber 100, and the reaction in the chamber 100. A control method for a film deposition apparatus 1000 that repeatedly supplies gas 300A and exhausts reaction gas 300A from chamber 100, wherein when raw material gas 200A is exhausted, the sixth valve 460 is closed and the cooling unit 610 is turned on, and when the raw material 200B collected in the cooling unit 610 reaches a predetermined amount, the heating unit 620 is turned on, and when regenerated raw material gas 200C is supplied from the regeneration mechanism 600 to chamber 100 via the return supply path 230, the third valve 430 and the fifth valve 450 are closed and the sixth valve 460 is opened.

[0093] According to this method, the heating unit 620 is turned on when the collected raw material 200B reaches a predetermined amount, making it possible to adjust the supply amount of recycled raw material gas 200C and control the purity and quality of the raw material gas 200A. In addition, the supply amount of recycled raw material gas 200C can be adjusted, for example, based on the application of the film to be formed.

[0094] Furthermore, in the control method of the film deposition apparatus 1000 of this embodiment, it is preferable to control the pressure of the regenerative raw material gas 200C based on the temperature and pressure of the regeneration mechanism 600 from the time the heating unit 620 is turned on until the regeneration raw material gas 200C is supplied from the regeneration mechanism 600 to the chamber 100. According to this method, since the pressure of the regenerative raw material gas 200C is controlled, the regenerative raw material gas 200C can be supplied into the chamber 100 quickly. Therefore, the cycle time can be shortened.

[0095] Furthermore, in the control method of the film deposition apparatus 1000 of this embodiment, when exhausting the raw material gas 200A from the chamber 100, it is preferable that the third valve 430 and the fifth valve 450 are opened and the sixth valve 460 is closed, thereby controlling the flow rate of the raw material gas 200A before it flows into the regeneration mechanism 600. According to this method, since the flow rate of the raw material gas 200A flowing into the regeneration mechanism 600 is controlled, the raw material gas 200A can be quickly exhausted from the chamber 100. Therefore, the cycle time can be shortened.

[0096] Furthermore, in the control method of the film deposition apparatus 1000 of this embodiment, the first valve 410 includes a first main valve 411 that controls the supply from the raw material gas storage section 200 to the chamber 100, and a first sub-valve 412 that controls the supply of regenerated raw material gas 200C to the chamber 100 via the return supply path 230. When the raw material gas 200A in the chamber 100 is exhausted via the raw material gas exhaust path 220, it is preferable that the first sub-valve 412 is in a closed state. With this method, since the first sub-valve 412 is in a closed state when the raw material gas 200A is exhausted, it is possible to suppress the flow of the generated regenerated raw material gas 200C into the chamber 100. Therefore, it is possible to suppress the mixing of raw material gas 200A and regenerated raw material gas 200C.

[0097] The following describes some variations of the embodiments described above.

[0098] As described above, the system is not limited to providing two third valves 430 and fourth valves 440, but may also be configured with a switchable, integrated valve, such as a three-way valve. Specifically, the three-way valve can be switched between exhausting the raw material gas 200A from the chamber 100 via the raw material gas exhaust path 220 and exhausting the reaction gas 300A from the chamber 100 via the reaction gas exhaust path 320.

[0099] Thus, in the control method of the modified film deposition apparatus 1000, it is preferable that the third valve 430 and the fourth valve 440 are integrated valves that can be switched between exhausting the raw material gas 200A from the chamber 100 via the raw material gas exhaust path 220 and exhausting the reaction gas 300A from the chamber 100 via the reaction gas exhaust path 320. With this method, since an integrated valve that can be switched, in other words, a valve such as a three-way valve is used, the exhaust path can be changed by controlling one valve.

[0100] As described above, the method is not limited to depositing an insulating film 32 on powdered metal particles 31; for example, the film may be deposited on a wafer instead of powder. Furthermore, the method is not limited to depositing an insulating film 32; a metal film, specifically aluminum, hafnium, tantalum, etc., may be deposited instead. [Explanation of symbols]

[0101] 31...Metal particles as material to be film-deposited, 32...Insulating film, 33...Particles with insulating film, 100...Chamber, 110...Pressure gauge, 200...Raw material gas storage section, 200A...Raw material gas, 200B...Raw material, 200C...Regenerated raw material gas, 210...Raw material gas supply path, 220, 221...Raw material gas exhaust path, 230...Return supply path, 250...Carrier gas storage section, 250A...Carrier gas, 251...Piping, 252...Valve, 253...Flow controller, 260...Carrier gas storage section, 260A...Carrier gas, 261...Piping, 261a...Spiral arrangement Pipe, 262... Valve, 263... Flow controller, 264... Valve, 300... Reaction gas storage section, 300A... Reaction gas, 310... Reaction gas supply path, 320... Reaction gas exhaust path, 410... First valve, 411... First main valve, 412... First sub-valve, 420... Second valve, 430... Third valve, 440... Fourth valve, 450... Fifth valve, 460... Sixth valve, 500... Suction pump, 600... Regeneration mechanism, 601... Tank, 610... Cooling section, 620... Heating section, 630... Pressure gauge, 640, 650... Collection amount detection sensor, 1000... Film deposition apparatus.

Claims

1. A chamber for housing the material to be treated with film deposition, A raw material gas storage unit is connected to the chamber and stores the raw material gas for forming a film on the film-forming member, A reaction gas storage unit connected to the chamber stores a reaction gas for reacting with the raw material gas, A regeneration mechanism comprising: a tank for containing the exhausted raw material gas; a cooling unit for cooling the raw material gas and collecting the raw material; a heating unit for sublimating the raw material to generate regenerated raw material gas; and a collection amount detection sensor for detecting the amount of the collected raw material. A suction pump for adjusting the pressure in the aforementioned tank, A return supply path for supplying the regenerating raw material gas from the regeneration mechanism to the chamber, A film deposition apparatus equipped with the following features.

2. A chamber for housing the material to be treated with film deposition, A raw material gas storage unit for storing raw material gas for forming a film on the member to be treated, A first valve for switching between supplying the raw material gas to the chamber or supplying recycled raw material gas that reuses the raw material gas, A reaction gas storage section for storing a reaction gas to be reacted with the raw material gas, A second valve that controls the supply of the reaction gas to the chamber, A raw material gas exhaust path is connected to the chamber and exhausts the raw material gas from the chamber via a third valve, A reaction gas exhaust path is connected to the chamber and exhausts the reaction gas from the chamber via a fourth valve, A suction pump for exhausting at least one of the raw material gas and the reaction gas from the chamber, A regeneration mechanism provided in the raw material gas exhaust path, having a cooling unit that collects raw materials contained in the raw material gas by cooling, and a heating unit that generates the regenerated raw material gas by sublimating the raw materials by heating, In the aforementioned raw material gas exhaust path, a fifth valve is provided between the regeneration mechanism and the suction pump, and is in an open state when the raw material gas is exhausted. A return supply path is connected between the regeneration mechanism and the first valve, and supplies the regeneration raw material gas back to the chamber via the sixth valve, Equipped with, A control method for a film deposition apparatus, comprising repeatedly supplying the raw material gas to the chamber and exhausting the raw material gas from the chamber, supplying the reaction gas to the chamber and exhausting the reaction gas from the chamber, When the raw material gas is exhausted, the sixth valve closes, and the cooling unit turns ON. When the amount of raw material collected in the cooling section reaches a predetermined amount, the heating section turns on. A control method for a film deposition apparatus, wherein when the regeneration raw material gas is supplied from the regeneration mechanism to the chamber via the return supply path, the third valve and the fifth valve are closed and the sixth valve is open.

3. A method for controlling a film deposition apparatus according to claim 2, A control method for a film deposition apparatus, comprising controlling the pressure of the regenerating raw material gas based on the temperature and pressure of the regeneration mechanism from the time the heating unit is turned on until the regeneration raw material gas is supplied from the regeneration mechanism to the chamber.

4. A method for controlling a film deposition apparatus according to claim 2, A control method for a film deposition apparatus, wherein when exhausting the raw material gas from the chamber, the third valve and the fifth valve are opened and the sixth valve is closed, thereby controlling the flow rate of the raw material gas before it flows into the regeneration mechanism.

5. A method for controlling a film deposition apparatus according to claim 2, The first valve includes a first main valve that controls the supply from the raw material gas storage unit to the chamber, and a first sub-valve that controls the supply of the regenerated raw material gas to the chamber via the return supply path. A control method for a film deposition apparatus, wherein the first sub-valve is closed when the raw material gas in the chamber is exhausted via the raw material gas exhaust path.

6. A method for controlling a film deposition apparatus according to claim 2, A control method for a film deposition apparatus, wherein the third valve and the fourth valve are integrated valves that can be switched between exhausting the raw material gas from the chamber via the raw material gas exhaust path and exhausting the reaction gas from the chamber via the reaction gas exhaust path.

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