Film forming apparatus, film forming method, and film formed body
The film forming apparatus and method address the challenge of forming uniform and dense films by using a circular cross-sectional aerosol transport path and controlled supply parameters, achieving stable and cost-effective film production with zirconia-based materials.
Patent Information
- Application Number
- JP2022512622
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Priority Date
- 2020-03-31
- Filing Date
- 2021-03-31
- Publication Date
- 2026-01-08
- Estimated Expiration
- 2041-03-31
AI Technical Summary
Existing film formation methods using aerosol deposition (AD) face challenges in achieving uniform and dense films, particularly with zirconia-based materials, due to issues with particle velocity control, nozzle design, and material accumulation, leading to porous regions and defects.
A film forming apparatus and method that utilizes an aerosol transport path with a circular cross-sectional area of 10 mm² at the ejection end and within the processing chamber, a distance of 100 mm or less to the substrate, and a supply rate of 1.5 to 30 g/min of ceramic raw material powder, along with a reduced processing chamber pressure of 0.6 kPa or less, to stabilize the aerosol flow and ensure uniform particle velocity.
This configuration allows for stable, long-term supply of ceramic raw material powder, forming a homogeneous and dense film by preventing particle accumulation and ensuring uniform particle velocity, thereby reducing production costs and defects.
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Abstract
Description
[Technical Field]
[0001] The present invention relates to a film forming apparatus and a film forming method for forming a film on a substrate, and a film formed body. [Background technology]
[0002] A method called aerosol deposition (AD) is a method for forming a film made of a metal oxide material on a substrate without undergoing high-temperature heat treatment such as sintering. In this AD method, raw material powder made of fine particles of metal oxide or the like is sprayed from a nozzle toward a substrate such as a ceramic or plastic at approximately the speed of sound, and the energy released when the raw material powder collides with the substrate causes the fine particles to fracture and deform, forming a film on the substrate.
[0003] As an apparatus used in the AD method, for example, a film formation apparatus described in Patent Document 1 has been proposed. The film formation apparatus described in Patent Document 1 includes an aerosol generating unit that generates an aerosol that is a mixture of raw material powder and a carrier gas, and a nozzle that injects the aerosol from an injection port, and can form a film on the substrate by injecting the aerosol from the injection port of the nozzle toward the substrate. [Prior art documents] [Patent documents]
[0004] [Patent Document 1] Japanese Patent Application Laid-Open No. 2007-246937 Summary of the Invention [Problem to be solved by the invention]
[0005] In the AD method, the impact force of the fine particles colliding with the substrate has a significant effect on the density of the film. Therefore, in order to obtain the desired uniform film quality, it is necessary to control the speed of the fine particles colliding with the substrate within an appropriate range. In particular, zirconia-based materials are highly hard and do not easily undergo brittle deformation when colliding with the substrate, and the process window in which they can be deposited is extremely narrow. Therefore, in order to form a uniform film, it is necessary to control the particle speed with high precision.
[0006] The film formation apparatus described in Patent Document 1 uses a nozzle with a small opening area and a throttle or a nozzle with a rectangular cross-sectional flow path. However, when a nozzle with a small opening area and a throttle is used, the carrier gas components of the aerosol are rapidly accelerated at the nozzle's outlet. Therefore, in the case of zirconia-based materials with a relatively high specific gravity, the particles cannot keep up with the acceleration of the carrier gas components and collide with the substrate at a low speed. This results in the generation of porous regions with low film density, making it difficult to obtain a dense film. Furthermore, when a nozzle with a rectangular cross-sectional flow path is used, the gas flow is easily disturbed at the rectangular edges, resulting in uneven gas velocity and ultimately uneven particle velocity, making it difficult to obtain a homogeneous film. Furthermore, when a nozzle with a relatively small opening area is used, the raw material powder is likely to accumulate inside the nozzle when a large amount of raw material powder is supplied over a long period of time. When the accumulated raw material powder is discharged, the fine particles are frequently not crushed or deformed when colliding with the substrate, resulting in the formation of a compact, which creates defects in the film and makes it unsuitable for mass production.
[0007] The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a film-forming apparatus, a film-forming method, and a film-formed body that can stably supply a large amount of ceramic raw material powder for a long period of time and form a uniform and dense film. [Means for solving the problem]
[0008] A characteristic configuration of a film forming apparatus according to the present invention for achieving the above object is a film forming apparatus for forming a film on a substrate, comprising: an aerosol generating unit that generates an aerosol in which ceramic raw material powder is dispersed in a gas; a raw material powder supply unit that supplies the ceramic raw material powder to the aerosol generating unit at a constant speed; a carrier gas supply means for supplying a carrier gas to the aerosol generating unit; an aerosol transport path through which the aerosol is ejected from a jetting end toward the substrate; a processing chamber in which at least a portion of the ejection end side of the aerosol transport path and the substrate are disposed in an internal space, The aerosol transport path has a flow path cross section at the ejection end with an area of 10 mm 2 End Circle It is a shape, The aerosol transport path has a cross section of a processing chamber transport portion located within the processing chamber having an area of 10 mm 2 End Circle It is a shape, the cross-sectional shape of the flow path in the transfer part within the processing chamber is the same as the cross-sectional shape of the flow path at the ejection end, The supply rate of the ceramic raw material powder supplied from the raw material powder supply unit to the aerosol generating unit is 1.5 to 30 g / min. Points is located. A characteristic configuration of a film forming method according to the present invention for achieving the above object is a method of forming a film on a substrate by generating an aerosol in an aerosol generating unit, the aerosol being a mixture of a carrier gas fed from a carrier gas feeding means and ceramic raw material powder fed from a raw material powder feeding unit, and ejecting the aerosol toward a substrate from an ejection end of an aerosol transport path, wherein: At least a portion of the ejection end side of the aerosol transport path and the substrate are disposed within an internal space of a processing chamber; The cross-sectional area of the aerosol transport path at the ejection end is 10 mm 2 End Circle It is a shape, The cross-sectional area of the flow path in the processing chamber transfer section located within the processing chamber is 10 mm 2 End Circle It is a shape, a supply rate of the ceramic raw material powder supplied from the raw material powder supply unit to the aerosol generation unit is 1.5 to 30 g / min, The aerosol is ejected toward the substrate from the ejection end of the aerosol transport path, the cross-sectional shape of which in the transport part inside the processing chamber is the same as the cross-sectional shape of the flow path at the ejection end. Points is located.
[0009] According to the above-mentioned characteristic configuration, the cross-sectional shape of the ejection end of the aerosol transport path A yen By using this shape, the flow rate of the aerosol at the ejection end becomes uniform within the cross section of the flow path. Therefore, a homogeneous and dense film can be formed on the substrate. In addition, the cross section of the flow path at the ejection end of the aerosol (the area of the cross section of the flow path) and the cross section of the flow path in the transport section inside the processing chamber are set to 10 mm 2 The cross-sectional shape of the flow path in the transfer part inside the processing chamber is the same as the cross-sectional shape of the flow path at the ejection end. Circle This shape significantly increases the cross-sectional area of the flow path at the ejection tip compared to conventional methods, making it difficult for ceramic raw material powder to accumulate inside the aerosol transport path, allowing for stable supply of large amounts of ceramic raw material powder for long periods of time. Furthermore, the increased cross-sectional area of the flow path gradually accelerates the gas components of the aerosol within the flow path, making it easier for particles to follow the acceleration of the gas, especially for zirconia-based raw material powder, which has a relatively high specific gravity. This makes it possible to collide particles with a sufficient velocity to form a dense film with the substrate. Furthermore, by setting the supply rate of the ceramic raw material powder from the raw material powder supply unit to the aerosol generation unit to 1.5 to 30 g / min, it is possible to shorten the time required to form a film with a desired thickness while avoiding problems such as pulsation in the raw material powder supply rate, which can prevent the formation of a uniform film, and increased manufacturing costs.
[0010] A further characteristic feature of the film formation apparatus and film formation method according to the present invention is that the distance from the ejection end of the aerosol transport path to the substrate is 100 mm or less.
[0011] Because the aerosol ejected from the ejection end of the aerosol transport path diffuses with a wide spread, the greater the distance from the ejection end of the aerosol transport path to the substrate, the larger the area of the film formed on the substrate. If the area formed on the substrate becomes large, when scanning the aerosol transport path or the substrate to obtain a uniform film, it is necessary to deposit a film over a larger area than the target film formation area. This increases the amount of raw material powder used, which may increase production costs. According to the above characteristic configuration, by keeping the distance from the ejection end of the aerosol transport path to the substrate at 100 mm or less, it becomes easier to suppress increases in production costs.
[0012] A further characteristic feature of the film forming apparatus and film forming method of the present invention is that the value obtained by dividing the area of the flow path cross section at the ejection end of the aerosol transport path by the square of the distance between the ejection end of the aerosol transport path and the substrate is 0.001 or more.
[0013] According to the above characteristic configuration, the value obtained by dividing the flow path cross-sectional area at the ejection end of the aerosol transport path by the square of the distance between the ejection end of the aerosol transport path and the substrate is 0.001 or more, which makes it less likely that variations will occur in the particle velocity in the direction perpendicular to the substrate when the substrate collides, thereby suppressing adhesion of the compact and the formation of pores and enabling the formation of a homogeneous film.
[0018] A further characteristic feature of the film forming apparatus and film forming method according to the present invention is that the pressure inside the processing chamber is set to 0.6 kPa or less.
[0019] The gas component of the aerosol rapidly decelerates and diffuses into the surroundings upon impact with the substrate, which may make it difficult for the particles affected to reach the substrate with sufficient speed. According to the above characteristic configuration, the viscosity of the gas component of the aerosol is reduced, making it difficult for the particles to be affected by the gas motion upon impact with the substrate, thereby enabling the formation of a denser and more uniform film.
[0020] A further characteristic feature of the film forming apparatus and film forming method according to the present invention is that the aerosol transport path is formed of a straight pipe member.
[0021] According to the above-described characteristic configuration, the aerosol transport path has a uniform cross-sectional shape throughout, which improves the flowability of the aerosol, reduces the likelihood of ceramic raw material powder accumulating, and enables a large amount of ceramic raw material powder to be stably supplied for a long period of time.
[0022] A further characteristic feature of the film-forming apparatus and film-forming method according to the present invention is that the density of the particles constituting the ceramic raw material powder is 4.0 g / cm 3 That's all there is to it.
[0023] According to the above characteristic configuration, the density is 4.0 g / cm 3 A homogeneous film can be formed from the ceramic raw material powder composed of the above particles.
[0024] A further characteristic feature of the film-forming apparatus and film-forming method according to the present invention is that the ceramic raw material powder is stabilized zirconia.
[0025] The inventors of the present invention have confirmed through experiments that a homogeneous film can be formed when stabilized zirconia is used as the ceramic raw material powder.
[0026] A feature of the film-formed body according to the present invention for achieving the above object is that it is formed by the above film-formation apparatus or the above film-formation method.
[0027] According to the above-described characteristic configuration, the film is formed by a film forming apparatus or a film forming method that can form a uniform and dense film, and therefore the film formed is uniform and dense. [Brief explanation of the drawings]
[0028] [Figure 1] 1 is a diagram showing the configuration of a film forming apparatus according to an embodiment of the present invention; [Figure 2] 1 is a view of the aerosol transport pipe according to the present embodiment as seen from the ejection end side. [Figure 3] FIG. 2 is a diagram showing the positional relationship between an aerosol transport pipe and a substrate. [Figure 4] FIG. 1 is a diagram showing the jetting end of a film forming apparatus used in Comparative Example 1. [Figure 5] FIG. 10 is a diagram showing the jetting end of the film forming apparatus used in Comparative Example 2. [Figure 6] FIG. 2 is a diagram schematically illustrating a substrate after a film formation treatment in Comparative Example 1. [Figure 7] FIG. 10 is a diagram schematically illustrating a substrate after a film formation treatment in Comparative Example 2. DETAILED DESCRIPTION OF THE INVENTION
[0029] DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS A film forming apparatus and a film forming method according to an embodiment of the present invention will be described below with reference to the drawings.
[0030] [About the film forming equipment] As shown in FIG. 1, the film forming apparatus according to this embodiment includes a processing chamber 2, an aerosol generating unit 6, an aerosol transport pipe 10 (aerosol transport path), a carrier gas supply means 15, and the like.
[0031] The processing chamber 2 is an airtight housing. The pressure inside the processing chamber 2 is reduced to a predetermined pressure (e.g., about 0.6 kPa) or less by exhausting gas using a mechanical booster pump 3 and a vacuum pump 4. The internal space of the processing chamber 2 also contains a holder 5 for holding a substrate K to be subjected to a film formation process, and a part of an aerosol transport pipe 10.
[0032] The aerosol generating unit 6 is a device that generates an aerosol in which ceramic raw material powder is dispersed in a gas. In this embodiment, the aerosol generating unit 6 is connected to a raw material powder supplying unit 7 via a raw material supplying pipe S1. The aerosol generating unit 6 is also connected to a carrier gas delivery pipe S2 and an aerosol transport pipe 10, which will be described later. The aerosol generating unit 6 generates an aerosol by mixing the ceramic raw material powder supplied at a constant rate from the raw material powder supplying unit 7 with a carrier gas delivered by a carrier gas delivery means 15. The generated aerosol is delivered to the aerosol transport pipe 10. Increasing the rate at which the ceramic raw material powder is supplied from the raw material powder supplying unit 7 to the aerosol generating unit 6 can shorten the time required to form a film with a target thickness. However, if the supply rate is too fast, pulsation occurs in the amount of raw material powder supplied, making it difficult to obtain a uniform film. On the other hand, if the supply rate is too slow, the film quality is improved, but the time required to complete film formation is lengthened, resulting in increased production costs. Therefore, the feed rate of the ceramic raw material powder is preferably 1.5 to 30 g / min.
[0033] As shown in FIGS. 1 to 3, the aerosol transfer pipe 10 is disposed in the processing chamber 2 such that its ejection end 10a and the processing chamber transfer section 10b (at least a portion of the ejection end side) face the holding section 5 in the processing chamber 2. The aerosol transfer pipe 10 in this embodiment is a cylindrical straight pipe member whose inner diameter has a predetermined flow path cross-sectional area A1 (the portion shown by the hatching in FIG. 3), and the end opposite the ejection end 10a is connected to the aerosol generation section 6. That is, in this embodiment, the flow path cross section at the processing chamber transfer section 10b and the flow path cross section at the ejection end 10a are both circular and have the same flow path cross-sectional area A1. Through this aerosol transfer pipe 10, aerosol is delivered from the aerosol generation section 6, and the delivered aerosol is delivered from the opening of the ejection end 10a.
[0034] Next, the flow path cross-sectional area A1 at the ejection end 10a of the aerosol transport pipe 10, the distance Ia between the ejection end 10a of the aerosol transport pipe 10 and the substrate K, and the relationship between the flow path cross-sectional area A1 and the distance Ia will be described.
[0035] The cross-sectional area A1 of the flow path at the ejection end 10a of the aerosol transport pipe 10 is 10 mm 2 There is no particular limitation as long as it is more than 20 mm. 2 It is preferable that it is 30 mm or more. 2 More preferably, it is 95 mm or more. 2 In this embodiment, the cross-sectional area A1 of the flow path is 95 mm 2 is.
[0036] Furthermore, the distance Ia from the ejection tip 10a of the aerosol transport pipe 10 to the substrate K is not particularly limited, but is preferably 100 mm or less, more preferably 40 mm or less, and even more preferably 10 mm or less. On the other hand, if the distance between the ejection tip 10a of the aerosol transport pipe 10 and the substrate K is too close and the substrate K has a distorted shape, there is a risk that the ejection tip 10a and the substrate K will come into contact when the aerosol transport pipe 10 and the substrate K are moved relative to each other. Therefore, the distance Ia between the ejection tip 10a of the aerosol transport pipe 10 and the substrate K is preferably 2 mm or more. In this embodiment, the distance Ia is 10 mm.
[0037] In the film forming apparatus 1, the cross-sectional area A1 of the flow path at the ejection end 10a of the aerosol transport pipe 10 is divided by the square of the distance Ia between the ejection end 10a of the aerosol transport pipe 10 and the substrate K (hereinafter, "(A1 / Ia 2 The value of (A1 / Ia) is set to be 0.001 or more (i.e., in this embodiment, 95 / 102 = 0.95). 2 Although the value of (A1 / Ia) is not particularly limited, it is preferably 0.001 or more, more preferably 0.007 or more, and even more preferably 0.03 or more. 2 ) value is preferably 25 or less, more preferably 1 or less.
[0038] The carrier gas supply means 15 includes a gas supply unit 16, a carrier gas pressure control unit 17, a carrier gas flow rate control unit 18, a carrier gas supply pipe S2, and the like.
[0039] Specifically, a carrier gas supply pipe S2 is connected to the gas supply unit 16, and the gas supply unit 16 supplies gases such as air, N2, He, and Ar into the carrier gas supply pipe S2 using a compressor or a gas cylinder.
[0040] In this embodiment, the carrier gas delivery pipe S2 is for delivering the gas supplied from the gas supply unit 16 as a carrier gas to the aerosol generation unit 6. Specifically, in this embodiment, the gas delivered from the gas supply unit 16 is delivered as a carrier gas to the aerosol generation unit 6 via the carrier gas pressure control unit 17 and the carrier gas flow rate control unit 18 in this order, and the carrier gas delivery pipe S2 is made up of a plurality of pipes connected between the gas supply unit 16, the carrier gas pressure control unit 17, the carrier gas flow rate control unit 18, and the aerosol generation unit 6. Furthermore, a pressure sensor P1 for detecting the pressure inside the carrier gas supply pipe S2 is provided between the carrier gas flow rate control unit 18 and the aerosol generating unit 6 in the carrier gas supply pipe S2.
[0041] The carrier gas pressure control unit 17 stabilizes the carrier gas flowing through the carrier gas supply pipe S2 at an appropriate pressure, and the carrier gas flow rate control unit 18 controls the flow rate of the carrier gas flowing through the carrier gas supply pipe S2. In this embodiment, the operations of the carrier gas pressure control unit 17 and the carrier gas flow rate control unit 18 are appropriately controlled based on the pressure detected by the pressure sensor P1, etc.
[0042] [About ceramic raw material powder] The particles constituting the ceramic raw material powder used in the film forming apparatus 1 have a density of 4.0 g / cm 3 The above particles are preferable, and examples of such particles are stabilized zirconia particles, which are zirconia containing yttrium, calcium, magnesium, hafnium, etc. In this embodiment, yttrium-containing zirconia (YSZ) is used as the ceramic raw material powder.
[0043] [Film formation method] Next, a process for forming a film (coated body) on a substrate K by a film formation method using the film formation apparatus 1 will be described. In the film formation method according to this embodiment, a carrier gas is fed from the gas supply unit 16 to the aerosol generation unit 6 while the flow rate and pressure of the carrier gas flowing through the carrier gas feed pipe S2 are adjusted by the carrier gas pressure control unit 17 and the carrier gas flow rate control unit 18. In the aerosol generation unit 6, an aerosol is generated in which the fed carrier gas is mixed with the ceramic raw material powder fed from the raw material powder supply unit 7. The generated aerosol is fed to the aerosol transfer pipe 10.
[0044] The aerosol fed to the aerosol transport pipe 10 is sprayed from the ejection end 10a of the aerosol transport pipe 10 toward the substrate K, and the sprayed aerosol collides with the substrate K to form a film on the substrate K.
[0045] Here, the aerosol ejected toward the substrate K is ejected from an ejection tip 10a having a circular flow path cross section, and the above (A1 / Ia 2 ) value is also 0.95 (i.e., 0.001 or more). Therefore, the velocity of the ejected aerosol is uniform within the flow path cross section of the ejection tip 10a, and there is little variation in the particle velocity in the direction perpendicular to the substrate K when it collides with the substrate K. Therefore, adhesion of the compacted powder and the formation of pores are suppressed, and a homogeneous and dense film is formed. In particular, when the ceramic raw material powder is stabilized zirconia such as YSZ, which has a relatively high density, a homogeneous film with high density can be formed. Furthermore, when the flow path cross section A1 of the ejection tip 10a is 95 mm 2 (i.e., 10 mm 2 As a result of the above, the ceramic raw material powder is less likely to accumulate at the ejection tip 10a, and a large amount of ceramic raw material powder can be supplied stably for a long period of time, making it possible to form a film on the substrate K over a long period of time.
[0046] Examples 1 to 5 and Comparative Examples 1 to 4 are explained below. The shape of the flow path cross section at the ejection end of the aerosol transport pipe, the flow path cross section area, and the distance between the ejection end and the substrate were changed, and the substrate was moved back and forth in a predetermined direction while a film formation process was carried out for a predetermined time. In each example and comparative example, the ceramic raw material powder had a density of 5.9 g / cm. 3 In each example and comparative example, the flow rate of the carrier gas was 18 L / min, and the pressure in the processing chamber was 0.2 kPa.
[0047] Tables 1 to 3 are tables summarizing the various conditions and results for Examples 1 to 5 and Comparative Examples 1 to 4, and the "area of the porous region" in Table 2 is the area of the porous region with low adhesion strength. 4 is a diagram showing the jetting end of the nozzle used in Comparative Example 1, and the area of the shaded portion A3 in the figure is the cross-sectional area of the flow path. The shape of the nozzle used in this Comparative Example 1 is the same as the shape of a nozzle conventionally adopted for a device that performs a film formation process using the AD method. Furthermore, Fig. 5 is a diagram showing the ejection tip of the nozzle used in Comparative Example 2, and the area of the shaded portion A2 in the figure is the cross-sectional area of the flow path. Also, Fig. 6 is a diagram showing a schematic view of the substrate after the film formation process in Comparative Example 1, and the direction of movement of the substrate is the up-down direction as one looks into the figure. Also, Fig. 7 is a diagram showing a schematic view of the substrate after the film formation process in Comparative Example 2, and as above, the direction of movement of the substrate is the up-down direction as one looks into the figure. In Figs. 6 and 7, the darkly shaded areas are the areas where the powder compact adheres.
[0048] [Table 1]
[0049] [Table 2]
[0050] [Table 3]
[0051] As can be seen from Table 1, when comparing Examples 1 and 2 with Comparative Examples 1 and 2, no adhesion of powder compacts was observed in Examples 1 and 2, whereas a large amount of powder compacts adhered to the substrate in Comparative Examples 1 and 2 (see Figs. 6 and 7). For example, as shown in Fig. 7, in Comparative Example 2, when the film formation process was performed while the substrate was moved back and forth, a large amount of powder compacts adhered to the portions where particles in the aerosol sprayed toward the substrate from corners where the aerosol flow is easily disturbed collided. From these findings, it was confirmed that by making the cross-sectional shape of the ejection end of the aerosol transport channel circular rather than rectangular or the conventional slit shape, the aerosol flow rate becomes uniform within the cross section of the channel, and a homogeneous film can be formed on the substrate.
[0052] Furthermore, as shown in Table 2, adhesion of the powder compact was not observed in Examples 3 to 5, in which the cross-sectional area of the flow path was slightly smaller than in Examples 1 and 2. On the other hand, in Examples 3 to 5, when attention was paid to the area of the porous region, (A1 / Ia 2 ) value is higher, the area of the porous region is smaller, and it can be seen that the homogeneity of the film is improved.
[0053] Furthermore, as shown in Table 3, in Comparative Examples 3 and 4, in which the flow path cross-sectional area was smaller than in Examples 3 to 5, a large amount of compact adhered to the substrate, even though the flow path cross-sectional shape was circular. This is presumably because, even if the flow path cross-sectional shape was circular, if the flow path cross-sectional area was too small, the raw material powder would clog. From this, it was confirmed that even if the flow path cross-sectional shape was circular, a certain amount of flow path cross-sectional area was necessary to suppress the formation of compact and form a uniform film on the substrate, and that if the flow path cross-sectional area was too small, a uniform film could not be formed on the substrate.
[0054] From the above, as in the film forming apparatus 1 and film forming method according to this embodiment, the aerosol transport pipe 10 has a flow path cross section at the ejection end 10a with an area of 10 mm 2It was confirmed that by using the above circular shape, it is possible to stably supply a large amount of ceramic raw material powder for a long period of time, and to form a homogeneous film.
[0055] [Other Embodiments] [1] In the above embodiment, the cross-sectional area A1 of the flow path at the ejection end 10a of the aerosol transport pipe 10 is 10 mm 2 Above and above, and above (A1 / Ia 2 ) value is 0.001 or more, but is not limited to this. 2 If it is more than (A1 / Ia 2 ) value does not have to be greater than 0.001.
[0056] [2] In the above embodiment, the distance from the ejection end 10a of the aerosol transport pipe 10 to the substrate K is 100 mm or less. 2 In particular, the cross-sectional area A1 of the flow path is 10 mm 2 and above (A1 / Ia 2 If the value of ) is 0.001 or more, the particle velocity in the direction perpendicular to the substrate when it collides with the substrate is less likely to vary, which has the effect of suppressing adhesion of the powder compact and the formation of pores.
[0057] [3] In the above embodiment, the aerosol transport pipe 10 is a cylindrical straight pipe member, but this is not limited thereto. Even if a separate crushing mechanism for crushing agglomerated particles or a classification mechanism for classifying particles is separately provided along the path of the straight pipe member, the aerosol flowability is not impaired, thereby achieving the effect of stably supplying a large amount of ceramic raw material powder for a long period of time. The aerosol transport pipe 10 does not need to be a straight pipe member as long as the shape of the flow path cross section at the ejection end 10a is approximately circular. Note that the term "approximately circular" includes not only perfect circles but also ellipses. Furthermore, the term "approximately circular" also includes triangles and polygons with pentagonal or greater corners with curved corners, and also includes quadrangles with curved corners where the ratio (r / R) of the radius r of the curved corner of the quadrangle to the radius R of the circumscribing circle is greater than 0.3. Even in such a case, the flow rate of the aerosol at the ejection end becomes uniform within the cross section of the flow path, which has the effect of enabling a homogeneous and dense film to be formed on the substrate.
[0058] [4] In the above embodiment, the flow path cross section at the processing chamber transfer part 10b of the aerosol transfer pipe 10 and the flow path cross section at the ejection end 10a are both circular with the same flow path cross-sectional area A1, but this is not limiting and the two shapes may be different. For example, the flow path cross section at the ejection end 10a may be circular and the flow path cross section at the processing chamber transfer part 10b may not be circular, or both flow path cross sections may be circular but have different areas. Note that the flow path cross-sectional area at the processing chamber transfer part 10b of the aerosol transfer pipe 10 is 10 mm 2 It is preferable that it is 20 mm or more. 2 More preferably, it is 30 mm or more. 2 More preferably, it is 95 mm or more. 2 More preferably, it is equal to or greater than this.
[0059] [5] In the above embodiment, the pressure inside the processing chamber is reduced to 0.6 kPa or less, but the present invention is not limited to this.
[0060] The configurations disclosed in the above embodiments (including other embodiments) can be applied in combination with configurations disclosed in other embodiments, as long as no contradictions arise. Furthermore, the embodiments disclosed in this specification are examples, and the embodiments of the present invention are not limited to these and can be modified as appropriate within the scope of the purpose of the present invention. [Industrial Applicability]
[0061] The present invention can be applied to a film forming apparatus and a film forming method for forming a film on a substrate, and a film-formed body. [Explanation of symbols]
[0062] 1: Film deposition equipment 10: Aerosol transport pipe (aerosol transport path) 10a: Spout end 10b: Transfer section inside the processing chamber K: Base material
Claims
1. A film forming apparatus for forming a film on a substrate, an aerosol generating unit that generates an aerosol in which ceramic raw material powder is dispersed in a gas; a raw material powder supply unit that supplies the ceramic raw material powder to the aerosol generating unit at a constant speed; a carrier gas supply means for supplying a carrier gas to the aerosol generating unit; an aerosol transport path through which the aerosol is ejected from a jetting end toward the substrate; a processing chamber in which at least a portion of the ejection end side of the aerosol transport path and the substrate are disposed in an internal space, The aerosol transport path has a flow path cross section at the ejection end with an area of 10 mm 2 It is circular as above, The aerosol transport path has a cross section of a processing chamber transport part located inside the processing chamber having an area of 10 mm 2 It is circular as above, the cross-sectional shape of the flow path in the transfer part within the processing chamber is the same as the cross-sectional shape of the flow path at the ejection end, a supply rate of the ceramic raw material powder supplied from the raw material powder supply unit to the aerosol generation unit being 1.5 to 30 g / min.
2. 2. The film forming apparatus according to claim 1, wherein the distance from the ejection end of the aerosol transport path to the substrate is 100 mm or less.
3. 3. The film forming apparatus according to claim 1, wherein a value obtained by dividing a cross-sectional area of the aerosol transport path at the ejection end by the square of a distance between the ejection end of the aerosol transport path and the substrate is 0.001 or more.
4. 2. The film forming apparatus according to claim 1, wherein the pressure in the processing chamber is set to 0.6 kPa or less.
5. 5. The film forming apparatus according to claim 1, wherein the aerosol transport path is formed of a straight pipe member.
6. The density of the particles constituting the ceramic raw material powder is 4.0 g / cm 3 The film forming apparatus according to any one of claims 1 to 5.
7. 7. The film forming apparatus according to claim 1, wherein the ceramic raw material powder is stabilized zirconia.
8. A method for forming a film on a substrate, comprising: generating an aerosol in an aerosol generating section, the aerosol being a mixture of a carrier gas delivered from a carrier gas delivery means and ceramic raw material powder delivered from a raw material powder supplying section; and ejecting the aerosol toward a substrate from an ejection end of an aerosol transport path, At least a portion of the ejection end side of the aerosol transport path and the substrate are disposed within an internal space of a processing chamber; The cross-sectional area of the aerosol transport path at the ejection end is 10 mm 2 It is circular as above, The cross-sectional area of the flow path in the processing chamber transfer part located within the processing chamber is 10 mm 2 It is circular as above, a supply rate of the ceramic raw material powder supplied from the raw material powder supply unit to the aerosol generation unit is 1.5 to 30 g / min, A film forming method in which the aerosol is ejected toward the substrate from the ejection end of the aerosol transport path, the cross-sectional shape of which in the transport section inside the processing chamber is the same as the cross-sectional shape of the flow path at the ejection end.
9. The film forming method according to claim 8, wherein the distance from the ejection end of the aerosol transport path to the substrate is 100 mm or less.
10. 10. The film forming method according to claim 8, wherein a value obtained by dividing a flow path cross-sectional area at the ejection end of the aerosol transport path by the square of a distance between the ejection end of the aerosol transport path and the substrate is 0.001 or more.
11. 9. The film forming method according to claim 8, wherein the pressure in the processing chamber is set to 0.6 kPa or less.
12. 12. The film forming method according to claim 8, wherein the aerosol transport path is formed of a straight pipe member.
13. The density of the particles constituting the ceramic raw material powder is 4.0 g / cm 3 The film forming method according to any one of claims 8 to 12.
14. 14. The film forming method according to claim 8, wherein the ceramic raw material powder is stabilized zirconia.
Citation Information
Patent Citations
Apparatus for forming composite structure
JP2004277826A
Film-forming apparatus and method for producing electronic parts
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