WO2007105670A1

WO2007105670A1 - Method for fabricating film-formed body by aerosol deposition

Info

Publication number: WO2007105670A1
Application number: PCT/JP2007/054778
Authority: WO
Inventors: Seiichi Yokoyama; Michiyori Miura
Original assignee: Hoya Corporation
Priority date: 2006-03-13
Filing date: 2007-03-12
Publication date: 2007-09-20
Also published as: JP2009132945A; TW200801237A

Abstract

There is provided a method for stably fabricating a film-formed body having a thick film by aerosol deposition. Raw material microparticles are sprayed from a plurality of nozzles toward a substantially identical area on a deposition substrate and the incident angle on the substrate is controlled, thereby forming the film-formed body while etching the deposited film.

Description

Specification

Method for producing film-forming body by aerosol deposition method

Technical field

[0001] The present invention relates to a method for forming a thick film-forming body using an aerosol deposition method.

Background art

[0002] The aerosol deposition method (hereinafter referred to as the AD method) is a ceramic having a particle size of several tens of nanometers to several μm, or a mixture of raw materials such as fine metal particle particles mixed with gas. In this technique, a film is formed by spraying onto a substrate through a nozzle. In recent years, the AD method has attracted attention as a method capable of forming a dense film having the same crystal structure as that of fine particles as a raw material at a low substrate temperature and at a high film formation rate.

A film forming apparatus using the AD method will be described with reference to FIG. FIG. 7 is a schematic diagram showing the basic configuration of the film forming apparatus. In the figure, 71 is a deposition substrate, 72 is an XY stage that moves the deposition substrate 71, 73 is a nozzle, 74 is a deposition channel, 75 is a classifier, 76 is an aerosol generator, and 77 is a high-pressure gas supply 78, a mass flow controller, 79 a pipeline, and arrows in the figure schematically indicate the substrate scanning direction. The raw material fine particles that also have ceramics or metal power are mixed with a carrier gas (not shown) supplied through the mass flow controller 78 inside the aerosol generator 76 to be aerosolized. The inside of the film forming chamber 74 is depressurized to about 50 Pa by a vacuum pump (not shown), and the raw material aerosolized by the gas flow generated by the pressure difference between this pressure and the pressure inside the aerosol generator 76. The fine particles are introduced into the film forming chamber 74 through the classifier 75 and sprayed to the film forming substrate 71 through the nozzle 73 at a high speed. The raw material particles transported by the gas are accelerated to several hundred mZs by passing through a nozzle with a fine opening of 1 mm or less.

[0004] The accelerated raw material fine particles collide with the deposition target substrate 71, and the kinetic energy is released at a stroke, so that a film is formed. However, even if all of the kinetic energy of the accelerated raw material fine particles is spent on raising the temperature of the raw material fine particles that have collided with the substrate, the temperature is, for example, an order of magnitude higher than the temperature necessary for sintering ceramics. Too low There are many unclear points regarding the mechanism by which a dense film is obtained. However, it is considered that the crushing generated when the raw material particles collide with the substrate plays an important role in the film formation process. “Fracture of the raw material fine particles” means both of the crushing of the raw material fine particles that have come to the substrate and the crushing of the raw material fine particles that have already adhered to the substrate surface.

[0005] That is, in Japanese Patent Application Laid-Open No. 2003-73855, in the case of raw material fine particles made of a brittle material, the average particle size of the fine particles is 50 nm or more, and the shape thereof is a non-spherical amorphous shape. As described above, it has been disclosed that by forming a shape with corners, the impact force at the time of substrate collision is concentrated on the corner portions, and the crushing of the raw material fine particles is promoted, resulting in a dense film formation. RU

Patent Document 1: Japanese Patent Laid-Open No. 2003-73855

Disclosure of the invention

Problems to be solved by the invention

[0006] However, as a result of systematic examination for forming a film-forming body having a large film thickness by our AD method, a film-forming body of about 10 m is formed relatively easily, but more than that It was found that it is difficult to stably form a film with a film thickness exceeding, for example, 30 m. That is, in the initial film formation process, in other words, in a thin film thickness of about 20 wm or less, a dense film body can be obtained, but as the film thickness increases, a dense film body is not formed. It became clear that there was a problem that only the green compact was formed. Means for solving the problem

[0007] In order to solve the above problems,

The first means provided by the present invention is:

The raw material fine particles are mixed with the carrier gas to form an aerosol, and together with the carrier gas, the raw material fine particles are accelerated through a plurality of nozzles arranged in parallel and sprayed toward the surface of the substrate to be deposited. In the aerosol deposition method for forming a film body, the raw material fine particles accelerated and jetted from the plurality of nozzles enter substantially the same location on the deposition surface of the deposition substrate and are accelerated and jetted from each nozzle. The incident direction of the raw material fine particles on the substrate to be deposited is different, and the substrate incident angle of the raw material fine particles that are accelerated and jetted from at least one of the plurality of nozzles is set to an angle at which the etching effect becomes apparent. A method for producing a film-forming body by an aerosol deposition method.

[0008] The second means provided by the present invention includes

The raw material fine particles are mixed with a carrier gas to form an aerosol, and together with the carrier gas, the raw material fine particles are accelerated through a plurality of nozzles arranged in parallel and sprayed toward the surface of the substrate to be deposited. In an aerosol deposition method for forming a film body, raw material particles accelerated and ejected from the plurality of nozzles are incident on substantially the same location on the deposition surface of the deposition substrate and are accelerated and ejected from each nozzle. The incident direction of the raw material fine particles to the substrate to be deposited is different, and the substrate incident angle of the raw material fine particles that are accelerated and jetted from at least one of the plurality of nozzles is set to an angle that exhibits only the etching effect. A method for producing a film-forming body by an aerosol deposition method.

[0009] The third means provided by the present invention includes

In the first or second means, the flow rate of the carrier gas containing the aerosolized raw material fine particles injected by at least one force of the plurality of nozzles, or the density force of the raw material fine particles in the carrier gas, etc. Nozzle force Manufacture of a film-forming body by the above-described aerosol deposition method, which is different from the flow rate of the carrier gas containing the aerosolized raw material fine particles or the concentration of the raw material fine particles in the carrier gas Is the method.

[0010] The fourth means provided by the present invention includes:

In any one of the first to third means, a carrier gas containing the aerosolized raw material fine particles is intermittently injected from at least one of the plurality of nozzles. It is a manufacturing method of a film body.

The fifth means provided by the present invention includes:

In any one of the first to fourth means, an angle formed by one of incident directions of the raw material fine particles accelerated and jetted from the plurality of nozzles on the deposition target substrate and a deposition target surface of the deposition target substrate is This is a method for producing a film-deposited body by the aerosol deposition method, characterized by being approximately 90 degrees.

Further, the sixth means provided by the present invention is

In any one of the first to fourth means, an incident direction of the raw material fine particles acceleratedly jetted from the plurality of nozzles to the deposition target substrate and a deposition target surface of the deposition target substrate are formed. A method for producing a film-formed body by an air sol deposition method, wherein at least one of the angles is substantially the same and the angle is 90 degrees or less.

The invention's effect

[0011] According to the present invention, it is possible to stably form a film-forming body having a high film thickness, for example, an ultra-thickness of 30 m, and excellent in denseness by using the AD method.

BEST MODE FOR CARRYING OUT THE INVENTION

[0012] The inventors have conducted extensive research to solve the above-mentioned problems, and have obtained the following knowledge. Hereinafter, the knowledge obtained by the inventors will be described.

[0013] As a result of observing, with an electron microscope, the structure of a film formed by the AD method, which is a dense film-forming body at the initial stage of film formation and becomes a green compact as the film thickness increases. Clearly, having an organization as shown schematically in Fig. 8 became a powerful force. FIG. 8 is a schematic diagram schematically showing a cross-sectional structure of a film formed under a condition where the carrier gas flow rate is constant, in which 81 is a substrate, 82 is a film formation layer, and 83 is a green compact layer. It is. In other words, the structure of the film formed by the raw material fine particles ejected from a single nozzle under the condition that the carrier gas flow rate is constant and the substrate incident angle of the raw material fine particles substantially coincides with the normal direction of the surface of the substrate 81. As shown in the figure, a dense film is formed in the film formation layer 82, and the diameter of the particles constituting the film formation layer 82 is about 1/10 to 1 of the particle diameter of the raw material fine particles. / 5. On the other hand, in the green compact layer 83, as the distance from the substrate 81 increases (as the film thickness increases), the number and size of voids increase, and the diameter of the particles constituting the green compact layer increases. As a result, it was clarified that the particle size of the raw material particles was about the same. It is also clear that the boundary between the film formation layer 82 and the green compact layer 83 is not clearly distinguishable, and the structural change from the film formation layer to the green compact layer occurs continuously. It was.

From this observation result, the cause of the formation of the green compact layer 83 is that the raw material fine particles are crushed as the film thickness is increased. It means that both the crushing of itself and the crushing of the raw material fine particles already attached to the substrate surface) are difficult to occur.

[0015] On the other hand, the cause of the crushing of the raw material fine particles is an impact force accompanying the release of the kinetic energy of the raw material fine particles at the time of the substrate collision, and the kinetic energy of the raw material fine particles is included. Lugi is determined by the substrate collision speed. By the way, when the carrier gas species is the same, the substrate collision speed of the raw material fine particles is determined by the flow rate of the carrier gas. The collision speed is always constant, and the kinetic energy released at the time of collision is also constant. Therefore, ideally, crushing of the raw material fine particles should occur as well regardless of the film thickness formed.

However, as described above, as a result of observing the cross-sectional structure of the film formed by the AD method with an electron microscope, as the film thickness increases, both the number of voids and the size thereof increase. It is assumed that the following phenomenon has occurred.

FIG. 9 is a diagram schematically showing the relationship between the pressure generated by the substrate collision of the raw material fine particles and the strain generated in the film forming body layer and the green compact layer. Generally, as shown in the figure, the pressure (stress) and strain increase linearly according to the pressure in the region where the pressure is low (in the figure, the elastic deformation region). The strain does not follow the pressure increase, and eventually breaks up (breaking point in the figure). In the green compact layer, since there are many voids, it is considered that the elastic deformation region that is easily deformed compared to the dense film formation layer is wide, and as a result, the pressure required for the occurrence of crushing (hereinafter referred to as the following) It is estimated that the critical pressure is also increasing. That is, when the pressure generated by the substrate collision of the raw material fine particles is lower than the critical pressure of the green compact layer exceeding the critical pressure in the film formation layer, and once the green compact layer is formed, the substrate The raw material fine particles adhering to the surface are not crushed, and the green compact layer continues to be formed.

[0018] In order to prevent the formation of the green compact layer, uncrushed raw material fine particles adhering to the substrate surface or fine particles that are not sufficiently crushed are used as the source of the green compact layer formation. It needs to be removed. Such uncrushed raw material fine particles or fine particles that are not sufficiently crushed are considered to have low adhesion to the surface of the substrate or the film formed on the substrate, and can be removed relatively easily. It is done.

That is, the present invention pays attention to the etching effect of the raw material fine particles incident on the substrate, which will be described below, and forms a dense film body while removing uncrushed raw material fine particles or fine particles that are not sufficiently crushed. It is something to be done. 4 to 6 show the influence of the incident direction of the raw material fine particles, in other words, the incident angle of the substrate.

[0021] FIG. 4a is a schematic diagram showing the relationship between the incident direction of the raw material fine particles and the substrate incident angle, in which 41 is the substrate, 42 is the film formed, 43 is the nozzle, 44 is the nozzle opening, and 45 is Raw material fine particles ejected from the nozzle opening 44. Figure 4b schematically shows the shape of the film formed for a fixed time with the substrate position fixed. In the figure, 46 is the shape of the film formation body, 47 is a uniform film thickness line, and P is the point where the thickest point is projected onto the substrate. When the substrate 41 is fixed and the raw material fine particles are sprayed toward the substrate surface for a certain period of time, the raw material fine particles 45 are incident on the substrate with a certain degree of directional distribution. It has a mountain shape as shown in the body 46. Here, the incident direction of the raw material fine particles is a direction parallel to a straight line connecting the point P and the center of the nozzle opening 44 and directed from the nozzle opening 44 to the point P. In general, it is understood as the direction indicated by the arrow shown in FIG. 4a and the block arrow. In addition, as shown in FIG. 4a, the substrate incident angle here means the angle between the substrate surface normal direction and the incident direction, Θ, and the angle between the deposition surface and the incident direction is ( 90—Θ) degrees.

FIG. 5 shows the relationship between the substrate incident angle and the film thickness of the film-deposited film formed for a certain period of time. The arrow in the figure corresponds to the case where the carrier gas flow rate is small, and the mouth mark corresponds to the case where the carrier gas flow rate is large. In both cases, the film thickness is standardized by the film thickness obtained when the film is formed with a substrate incident angle of 0 degrees (that is, the angle between the deposition surface and the incident direction of the raw material fine particles is 90 degrees). As shown in the figure, when the substrate incident angle exceeds 20 degrees, the film thickness of the film formation starts to decrease sharply, and when the carrier gas flow rate is small, the decrease amount is when the flow rate is large. Smaller than that. It is estimated that this is because the etching effect of particles incident on the substrate becomes obvious as the substrate incident angle increases. In addition, the magnitude of the etching effect depends on both the substrate incident angle and the carrier gas flow rate. From this, the incident angle at which the etching effect becomes apparent changes depending on the carrier gas flow rate.

[0023] FIG. 6 shows the relationship between the amount of decrease in film thickness and the incident angle of the substrate after the raw material fine particles are incident on the substrate for a certain period of time after forming the film-forming body having a certain thickness. It is. As in Fig. 5, the arrow in the figure corresponds to the case where the carrier gas flow rate is small, and the mouth mark corresponds to the case where the carrier gas flow rate is large. Also, in the figure, when the film thickness reduction amount is 0, no film thickness reduction occurs. And when the raw material fine particles incident on the substrate are deposited and the film thickness is increased.

[0024] As shown in the figure, when the carrier gas flow rate is large, the decrease in film thickness becomes apparent when the substrate incident angle exceeds 25 degrees, whereas when the carrier gas flow force is small, the substrate The decrease in film thickness becomes apparent when the incident angle exceeds 40 degrees (hereinafter, the angle at which the film thickness phenomenon becomes apparent is referred to as “the angle at which only the etching effect appears”). The angle at which only the etching effect appears depends on both the substrate incident angle of the raw material fine particles and the carrier gas flow rate.

From the above results, it is understood that the etching effect of the raw material fine particles can be controlled by appropriately selecting the substrate incident angle of the raw material fine particles and the carrier gas flow rate in the AD method.

[0026] The present invention has been made based on the above-mentioned knowledge obtained by the inventors. That is, according to the present invention, by forming a film using a plurality of nozzles, the above-described etching effect and the deposition effect are harmonized, and the unadhered to the substrate surface, which is the source of the formation of the green compact layer. While removing raw material fine particles for crushing or fine particles that are not sufficiently crushed, a film formed with a large film thickness and excellent density is formed.

Hereinafter, embodiments of the present invention will be described.

1 to 3 are schematic views showing an embodiment of the present invention, and schematically show the relationship between a substrate position and a nozzle.

FIG. 1 schematically shows a case where a film-forming body is formed by raw material fine particles ejected from the first and second nozzle caps. In the figure, 11 is the first nozzle, 12 is the second nozzle, 13 is the raw material fine particles that are also injected with the first nozzle force, and 14 is the raw material fine particles that are injected from the second nozzle. In addition, the arrows and block arrows in the figure indicate the incident directions of the raw material fine particles 13 and 14 on the substrate. In the configuration shown in the figure, the incident direction of the raw material fine particles 13 is substantially parallel to the normal of the substrate surface (the substrate incident angle is approximately 0 degrees), and is mainly responsible for the formation of the film formation body 42. On the other hand, the raw material fine particles 14 mainly have a function of removing uncrushed raw material fine particles adhering to the surface of the film formation body or particles that are not sufficiently crushed, so that the incident direction is limited to the normal of the substrate surface. (The substrate incident angle is not zero), and the value is the angle at which the etching effect is manifested (the “etching effect is manifested” here) However, it does not mean that film deposition does not occur at all, but it means that the deposition rate starts to decrease, and the “angle at which the etching effect becomes apparent” is the above-mentioned “only the etching effect”. The “incident angle” is a substrate incident angle in which both the etching effect and the film deposition effect coexist. For example, the substrate incident angle is an angle of about 20 degrees or more. The same shall apply hereinafter. Further, the substrate collision speed of the raw material fine particles ejected from the nozzles 11 and 12, in other words, the carrier gas flow rate, or the concentration of the raw material fine particles in the carrier gas is a condition that a dense film formation 42 is formed. Can be selected as appropriate. Further, it is possible to select the same for the force for continuously injecting the raw material fine particles from each of the nozzles 11 and 12 or intermittently.

FIG. 2 schematically shows a case where a film-forming body is formed by the raw material fine particles that are ejected by the first, second, and third nozzle forces. In the figure, 21 is the first nozzle, 22 is the second nozzle, 23 is the third nozzle, 24 is the raw material particles injected from the first nozzle, 25 is the raw material particles injected from the second nozzle, 26 is a raw material fine particle injected from the third nozzle cover. In addition, the arrows and block arrows in the figure indicate the substrate incident directions of the respective raw material fine particles 24, 25, and 26.

[0030] The configuration shown in the figure corresponds to the configuration of the nomination of the configuration shown in FIG. That is, the incident direction of the raw material fine particles 24 is substantially parallel to the normal line of the substrate surface (substrate incident angle is approximately 0 degrees), and is mainly responsible for the formation of the film formation body 42. On the other hand, since the raw material fine particles 25 and 26 mainly have a function of removing uncrushed raw material fine particles adhering to the surface of the film forming body or particles that are not sufficiently crushed, the incident direction is the normal line of the substrate surface. A finite angle is formed, and the value is set to an angle at which the etching effect becomes apparent. In addition, the dense film formation 42 is formed according to the substrate collision speed of the raw material fine particles injected from each nozzle 21, 22, 23, in other words, the carrier gas flow rate, or the concentration of the raw material fine particles in the carrier gas. This can be selected as appropriate. In addition, it is possible to select the same for the nozzle 21, 22, 23 from which the raw material fine particles are sprayed continuously or intermittently.

FIG. 3 schematically shows a case where a film-forming body is formed by raw material fine particles ejected from the first and second nozzle caps. In the figure, 31 is the first nozzle, 32 is the second nozzle , 33 is a raw material fine particle that is also injected by the first nozzle force, and 34 is a raw material fine particle that is injected from the second nozzle. In addition, the arrows and block arrows in the figure indicate the incident directions of the raw material fine particles 33 and 34 on the substrate. The configuration shown in the figure has the same force as the configuration shown in FIG. 1 in that the first and second nozzle forces are configured. The substrate incident direction of the raw material fine particles 33 and the raw material fine particles 34 However, they are different in that both form a certain angle with the normal of the substrate surface. In this configuration, the substrate incident angle of the raw material fine particles 33 and 34 is clearly recognized as an etching effect, but the film deposition effect is excellent (for example, the substrate incident angle is in the range of 20 to 30 degrees). The film forming body is formed while etching is performed. Of course, it is possible to form a film-forming body while performing etching with one nozzle. However, in such a case, the film-forming speed decreases, and it is not suitable as a method for forming a particularly thick film. In addition, in some cases, raw material fine particles having a force only in one direction may not be uniformly etched by the already formed film particles. Therefore, if the number of nozzles is increased to 2 or more in the configuration shown in FIG. 3, a relatively thick film can be formed in a relatively short time.

Hereinafter, embodiments of the present invention will be described in more detail using examples.

Example 1

[0033] Alumina particles having an average particle diameter of 0.7 μm were used as raw material fine particles, and air was used as a carrier gas. The substrate and nozzle arrangement are substantially the same as those shown in FIG. The first nozzle (corresponding to the nozzle 11 in FIG. 1) force of the alumina fine particles (corresponding to the raw material fine particles 13 in FIG. 1) is also injected with a substrate incident angle of approximately 0 degrees, The substrate incident angle of alumina fine particles (corresponding to raw material fine particles 14 in FIG. 1) ejected from the nozzle (corresponding to nozzle 12 in FIG. 1) was set to approximately 30 degrees. The nozzle openings of the first and second nozzles are both 5 nm × 0.3 nm, and the substrate used is quartz glass. The gas flow rate injected from the first and second nozzles was both set to 3 lZmin. At this time, the substrate collision speed of the alumina fine particles into which the first and second nozzle forces were also injected was 220 mZs, and the obtained film formation speed was ˜5 mZmin. During film formation, the above-described carrier gas flow rate was maintained, and an aluminum film formation body having a film thickness of ˜30 m was formed.

As a comparative example, the first nozzle (corresponding to nozzle 11 in FIG. 1) Although we attempted to form a film only with lumina fine particles (corresponding to raw material fine particle 13 in Fig. 1), formation of a green compact was observed from around the film thickness force S 15 m. It could not be formed.

Example 2

[0035] Under the same conditions as in Example 1, an alumina film-forming body having a thickness of up to 30 μm was formed. However, the carrier gas flow rate at which the force of the first nozzle (corresponding to nozzle 11 in FIG. 1) is also injected is a force of 3 lZmin, as in Example 1. In this example, the second nozzle ( The flow rate of the carrier gas injected from the nozzle 12 in FIG. 1 was set to 5 lZmin. At this time, the substrate collision speed of the alumina fine particles injected from the second nozzle was 300 mZs, and the film formation speed obtained was ˜3 / z mZmin. During the film formation, the above-described carrier gas flow rate was maintained to form a 30 m thick alumina film.

Example 3

[0036] Under the same conditions as in Example 2, a 40 μm-thick alumina film was formed. However, the carrier gas flow rate at which the first nozzle (corresponding to nozzle 11 in FIG. 1) force is also injected is a force of 3 lZmin, as in Example 2. In this example, the second nozzle ( The carrier gas type injected from the nozzle 12 in FIG. 1 is He, and its flow rate is 4 lZmin. At this time, the substrate collision speed of the alumina fine particles injected from the second nozzle was 450 m / s, and no alumina film deposition was observed.

[0037] In this example, the alumina fine particles were ejected intermittently from the second nozzle while the alumina fine particles were continuously ejected from the first nozzle. Figure 10 shows the injection scheme. In other words, every two minutes, alumina fine particles having a thickness of ˜40 / ζ πι were formed by repeating a cycle of spraying alumina fine particles from the second nozzle cover for about 20 seconds. .

Example 4

[0038] Under approximately the same conditions as in Example 3, an alumina film-forming body having a thickness of -30 μm was formed. However, in the case of the present example, both the first and second nozzles were intermittently sprayed with alumina fine particles formed therefrom. Figure 11 shows the injection scheme. In other words, after the alumina fine particles are injected from the first nozzle for ² minutes, the injection is stopped, and then the second nozzle for about 20 seconds. By repeating the cycle of spraying alumina fine particles, a 30 m thick alumina film was formed.

Example 5

[0039] Alumina particles having an average particle size of 0.7 μm were used as raw material fine particles, and air was used as a carrier gas. The substrate and nozzle arrangement are substantially the same as those shown in FIG. The substrate incident angle of the alumina fine particles (corresponding to the raw material fine particles 24 in FIG. 2) ejected from the first nozzle (corresponding to the nozzle 21 in FIG. 2) is approximately 0 degrees, and the second nozzle (in FIG. 2). The substrate incident angle of alumina fine particles (corresponding to raw material fine particles 25 in Fig. 2) injected from the nozzle 22) is approximately 30 degrees, and is injected from the third nozzle (corresponding to nozzle 23 in Fig. 2). The substrate incident angle of alumina fine particles (corresponding to raw material fine particles 26 in FIG. 2) was set to approximately 30 degrees. The substrate incident angles of the alumina fine particles injected from the second and third nozzle caps have substantially the same absolute values and different signs (ie, the angles are substantially the same but the incident directions are different). The nozzle openings of the first, second, and third nozzles are all 5 nm × 0.3 nm, and the substrate used is quartz glass. In addition, the gas flow rates injected from the first, second and third nozzles were both set to 3 lZmin. At this time, the substrate collision speed of the alumina fine particles injected from the first, second, and third nozzles was 220 mZs, and the obtained film formation speed was ˜7 mZmin. During the film formation, the carrier gas flow rate described above was maintained, and an alumina film body having a thickness of ˜30 μm was formed.

Example 6

[0040] Alumina particles having an average particle diameter of 0.7 μm were used as raw material fine particles, and air was used as a carrier gas. The substrate and nozzle arrangement are substantially the same as those shown in FIG. The substrate incident angle of the alumina fine particles (corresponding to the raw material fine particles 33 in FIG. 3) ejected from the first nozzle (corresponding to the nozzle 31 in FIG. 3) is about 30 degrees, and the second nozzle (nozzle in FIG. 3). The substrate incident angle of alumina fine particles (corresponding to raw material fine particles 34 in Fig. 3) ejected from (corresponding to 32) was set to approximately 30 degrees. The substrate incident angles of the alumina fine particles ejected from the first and second nozzles are substantially the same in absolute value and different in sign (ie, the angles are substantially the same but the incident directions are different). The nozzle openings of the first and second nozzles are both 5 nm × 0.3 nm, and the substrate used is quartz glass. Also, the first and second nozzles spray Both gas flow rates were set to 3 lZmin. At this time, the substrate collision speed of the alumina fine particles to which the first and second nozzle forces were also injected was 220 mZs, and the obtained film formation speed was ˜3 mZmin. During the film formation, the carrier gas flow rate described above was maintained, and an alumina film body having a thickness of ˜30 μm was formed.

[0041] Although the present invention has been described in detail with reference to the examples, the present invention is not limited to the above-described transport gas type, flow rate, transport gas injection scheme, or raw material fine particle material, and the number of nozzles. It is not limited to the substrate incident angle of the raw material fine particles.

Industrial applicability

[0042] The film forming method according to the present invention is useful for forming a thick film-forming body using the AD method, and industrial fields relating to parts and materials using the film-forming body. It is available in

Brief Description of Drawings

FIG. 1 is a schematic diagram showing the relationship between a substrate position and a nozzle.

FIG. 2 is a schematic diagram showing a relationship between a substrate position and a nozzle.

FIG. 3 is a schematic diagram showing a relationship between a substrate position and a nozzle.

FIG. 4 is a schematic diagram for explaining a substrate incident angle.

FIG. 5 is a diagram showing the relationship between the film thickness of a film-formed body and the substrate incident angle.

FIG. 6 is a diagram showing the relationship between the film thickness reduction amount and the substrate incident angle.

FIG. 7 is a schematic diagram showing a basic configuration of a film forming apparatus using the AD method.

FIG. 8 is a schematic view schematically showing a cross-sectional structure of a sample formed by the AD method.

FIG. 9 is a diagram schematically showing the relationship between the pressure generated by substrate collision of raw material fine particles and the strain generated in the film formation layer and the green compact layer.

FIG. 10 shows a carrier gas injection scheme.

FIG. 11 shows a carrier gas injection scheme.

Explanation of symbols

[0044] 11 First nozzle

12 Second nozzle

13 First nozzle force Raw material particles to be injected Raw material particles that are also injected with the second nozzle force First nozzle

Second nozzle

3rd nozzle

Raw material fine particles that are also injected with the first nozzle force Second nozzle force Raw material fine particles that are injected Second nozzle force Raw material fine particles that are injected Third nozzle force Raw material fine particles that are injected First nozzle

Second nozzle

1st nozzle force Raw material fine particles to be injected 2nd Nozzle force raw material fine particles to be injected Substrate

Deposited film

Nozzle

Nozzle opening

Raw material fine particles sprayed from nozzle opening 44 Shape of film formation

Equal film thickness

Deposition substrate

XY stage

Nozzle

Deposition chamber

Classifier

Aerosol generator

High pressure gas supply source

Mass flow controller

pipeline 81 board

82 Deposition layer

83 Green compact layer

P Point where the thickest point is projected onto the substrate

Claims

The scope of the claims

[1] Raw material fine particles are mixed with a carrier gas to form an aerosol, and together with the carrier gas, the raw material fine particles are accelerated through a plurality of nozzles arranged in parallel and sprayed toward the surface of the substrate to be deposited. An aerosol deposition method for forming a film-forming body in

The raw material particles accelerated and ejected from the plurality of nozzles enter substantially the same location on the surface of the substrate to be deposited, and the incident directions of the raw material particles accelerated and ejected from the nozzles on the substrate to be deposited are different. In addition, the substrate incident angle of the raw material fine particles accelerated and ejected from at least one of the plurality of nozzles is set to an angle at which the etching effect becomes apparent. .

[2] The raw material fine particles are mixed with the carrier gas to be aerosolized, and together with the carrier gas, the raw material fine particles are accelerated through a plurality of nozzles arranged in parallel and ejected toward the surface of the substrate to be deposited. An aerosol deposition method for forming a film-forming body in

The raw material particles accelerated and ejected from the plurality of nozzles enter substantially the same location on the surface of the substrate to be deposited, and the incident directions of the raw material particles accelerated and ejected from the nozzles on the substrate to be deposited are different. In addition, the substrate incidence angle of the raw material fine particles accelerated and ejected from at least one of the plurality of nozzles is set to an angle at which only the etching effect appears, and the method for producing a film-forming body by the aerosol deposition method .

[3] The flow rate of the carrier gas containing the aerosolized raw material fine particles or the density of the raw material fine particles in the carrier gas injected from at least one of the plurality of nozzles is injected from other nozzles. 3. The production of a film-forming body by the aerosol deposition method according to claim 1, wherein the flow rate of the carrier gas containing the aerosolized raw material fine particles is different from the concentration of the raw material fine particles in the carrier gas. Method.

[4] The air port according to any one of claims 1 to 3, wherein the carrier gas containing the aerosolized raw material fine particles is intermittently ejected at least once by the plurality of nozzles. A method for producing a film-formed body by a sol deposition method.

[5] The direction of incidence of the raw material fine particles sprayed from the plurality of nozzles on the deposition target substrate 5. The method of forming a film-forming body by the aerosol deposition method according to claim 1, wherein an angle between the surface of the substrate to be deposited and a deposition surface of the deposition substrate is approximately 90 degrees. At least one of the incident direction of the raw material fine particles acceleratedly jetted from the plurality of nozzles to the deposition target substrate and the deposition target surface of the deposition target substrate is substantially the same, and the angle is 90 degrees or less. The method for producing a film-forming body by the aerosol deposition method according to any one of claims 1 to 4.