JP2008231552A - Nozzle for jetting aerosol, and film deposition apparatus equipped therewith, and film deposition method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a film deposition apparatus in which the grain size distribution, particle velocity or particle concentration of an aerosol flow in an aerosol deposition method can be exactly measured by using a laser, and a film deposition method. <P>SOLUTION: The nozzle for jetting the aerosol used in the aerosol deposition method includes an aerosol introducing opening, an aerosol exit opening, and an aerosol flow passage for passing the aerosol from the introducing opening to the exit opening. An inner peripheral wall surface delineating the aerosol flow passage is provided with a laser exit surface and a laser photodetecting surface. The laser exit surface is a surface to emit the laser of a laser irradiation apparatus, from which surface the laser is emitted into the aerosol flow passage. The laser photodetecting surface is the photodetecting surface of a sensor detecting the physical quantity of the laser and receives the laser emitted from the laser exit surface. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to an aerosol injection nozzle used in an aerosol deposition method, and a film forming apparatus and a film forming method using the same.

  In recent years, the aerosol deposition method has attracted attention as a method for forming a ceramic thin film used as a piezoelectric actuator or the like. In this method, an aerosol formed by dispersing ceramic fine particles in a gas is sprayed from a nozzle and sprayed onto the substrate surface at a high speed, whereby fine particles are pulverized and deposited on the substrate to form a ceramic thin film. This method utilizes the phenomenon of normal temperature impact solidification of ceramic fine particles, and eliminates the need for the sintering process at 1000 ° C. or higher, which has been performed in the conventional ceramic thin film forming method. Therefore, it is not necessary to design a thin film in consideration of dimensional accuracy, and a fine nanocrystal structure is formed by crushing fine particles, and a ceramic thin film having an extremely smooth surface can be manufactured.

  In the aerosol deposition method, in the process of film formation, the reduction of fine particles in the aerosol generator, the fluctuation of the flow rate of the carrier gas, the formation of agglomerated huge particles due to the aggregation of fine particles, the aerosol supply pipe and the injection The particle size distribution, particle velocity, or particle concentration of the aerosol flow injected from the nozzle may vary over time due to various factors such as clogging of the nozzle and the like. However, when these fluctuate, the thickness of the resulting ceramic thin film becomes uneven, which adversely affects its performance. In order to maintain a uniform film pressure and consequently performance of the ceramic thin film, the particle size distribution, particle velocity, or particle concentration of the aerosol flow is measured in real time, and the aerosol generation conditions and spraying conditions are controlled according to the results. It is desirable to do.

  In general, the particle size distribution of an aerosol is measured by using a commercially available laser diffraction / scattering particle size distribution measuring apparatus. This device measures the intensity distribution of the diffracted / scattered light obtained by irradiating the aerosol with a laser, and calculates the particle size distribution by converting the measurement results using Mie's scattering theory or Fraunhofer's diffraction theory. (See, for example, Patent Document 1). Since this apparatus only requires a very short time, it is suitable for measuring the particle size distribution of the aerosol in real time during film formation by the aerosol deposition method.

  For the aerosol particle concentration, use the above laser diffraction / scattering particle size distribution measuring device to obtain the total intensity of the light diffracted / scattered by the aerosol, and obtain the aerosol with a known concentration in advance as the measurement target. It can be calculated in comparison with the measurement result of the diffracted / scattered light intensity (see, for example, Patent Document 2).

  It is known that the aerosol particle velocity can be calculated by a laser Doppler velocimeter utilizing the Doppler effect (see, for example, Patent Document 3). In this method, since the scattered light obtained by irradiating the aerosol with the laser has a wavelength that is influenced by the particle velocity of the aerosol due to the Doppler effect, the wavelength of the aerosol is compared with the wavelength of the incident laser and the wavelength of the scattered light. The particle velocity is obtained.

As described in Patent Document 3, conventionally, measurement of the aerosol particle velocity and the like in the aerosol deposition method has been performed by irradiating a laser beam to the aerosol flow ejected from the ejection nozzle.
JP 2005-61941 A JP 2000-46722 A JP 2007-31737 A

  In the aerosol deposition method, not all ceramic fine particles sprayed on the substrate surface as an aerosol flow are consumed for forming a thin film. Most of the ceramic fine particles collide with the substrate surface, and then are crushed and repelled without contributing to the formation of the thin film, and are scattered and floated in the atmosphere in the chamber. In many cases, the fine particles floating in the chamber come into contact with and adhere to various members in the chamber.

  Therefore, when measuring the particle size distribution or particle velocity of the aerosol flow after irradiating the aerosol flow after being ejected from the injection nozzle, in addition to the fine particles contained in the aerosol flow that is the measurement target, It is difficult to accurately measure suspended particles that are not.

  In addition, if suspended fine particles adhere to the laser emitting surface and the light receiving surface, this causes a problem that the laser and diffracted / scattered light to be received are scattered, thereby reducing the measured light intensity. Since the measurement of the particle concentration is based on the light intensity of the diffracted / scattered light, it is difficult to accurately measure the particle concentration.

  Therefore, the present invention has an object to provide a film forming apparatus and a film forming method capable of accurately measuring the particle size distribution, particle velocity, or particle concentration of an aerosol flow in an aerosol deposition method using a laser. And

  This invention is made | formed in view of the said present condition, and solves the said subject by incorporating a laser emitting surface and a laser light-receiving surface inside the nozzle for aerosol injection.

  That is, an aerosol injection nozzle according to the present invention includes an aerosol injection including an introduction opening for introducing aerosol, an injection opening for injecting aerosol, and an aerosol flow path for allowing the aerosol to pass from the introduction opening to the injection opening. A laser emitting surface and a laser light receiving surface provided on an inner peripheral wall surface defining the aerosol flow path, and the laser emitting surface is a surface for emitting a laser of a laser irradiation device, from which A laser is emitted into the aerosol flow path, and the laser light receiving surface is a light receiving surface of a sensor that detects a physical quantity of the laser, and receives the laser emitted from the laser emitting surface.

  In a conventional deposition apparatus using the aerosol deposition method, a laser emitting surface and a laser receiving surface are arranged outside the injection nozzle, and the aerosol flow after being ejected from the injection nozzle is irradiated with a laser so that the particle size distribution, etc. In the present invention, the laser emitting surface and the laser light receiving surface are arranged on the inner wall surface of the injection nozzle to irradiate the aerosol flow flowing in the injection nozzle with the laser, and the material in the aerosol flow is measured. Only light diffracted and scattered by particles is detected. Since the aerosol flow is ejected from the injection nozzle at a high speed, the material particles floating in the chamber do not flow back into the injection nozzle. Therefore, only diffracted / scattered light caused by material particles in the aerosol flow can be detected, noise caused by diffracted / scattered light generated from suspended material particles can be eliminated, and the particle size distribution and particle velocity of the aerosol flow can be accurately determined. It becomes possible to measure.

  In the aerosol injection nozzle according to the present invention, a part of the inner peripheral wall surface is a tapered portion formed so as to reduce a cross-sectional area of the aerosol flow path as going downstream, and the inner peripheral wall surface It is preferable that the laser emitting surface and the laser receiving surface are provided in a portion downstream of the taper portion.

  By doing so, the aerosol flow passing through the injection nozzle is accelerated because the cross-sectional area of the aerosol flow is reduced by the tapered portion, and in the accelerated state, the aerosol flow is jetted from the injection nozzle and sprayed onto the substrate. . The higher the aerosol flow speed, the more the material particles are prevented from adhering to the peripheral members. By providing a laser emitting surface and a laser receiving surface downstream of the tapered portion, the laser emitting surface and the laser receiving surface are provided. The adhesion of material particles to the surface can be prevented, and the particle concentration of the aerosol flow can be accurately measured. Moreover, since the particle size distribution, particle velocity, and particle concentration of the final aerosol flow sprayed on the substrate are measured, the obtained measurement results can be effectively used by homogenizing the thin film to be manufactured.

  In the present invention, the inner peripheral wall surface includes a pair of parallel flat portions facing each other across the central axis of the aerosol flow path, and the laser emitting surface and the laser receiving surface are provided on the flat portion. It is preferable.

  Here, since the direction of the central axis of the aerosol flow path is parallel to the flow direction of the aerosol flow, in the above configuration, the flow direction of the aerosol flow is parallel to the laser emission surface and the laser light receiving surface. Become. With this configuration, the material particles in the aerosol flow are less likely to adhere to the laser emitting surface and the laser receiving surface.

  In the present invention, it is preferable that a laser is emitted from the laser emission surface in a direction oblique to the central axis of the aerosol flow path.

  In this way, since the flow direction of the aerosol flow and the traveling direction of the laser cross at an angle, the particle velocity can be measured based on the laser Doppler method.

  In the present invention, it is preferable that the laser emitting surface and / or the laser receiving surface is constituted by an optical fiber cross section.

  With this configuration, it becomes easy to incorporate a laser emitting surface and a laser receiving surface into a minute size nozzle. Further, if the cross section is connected to a laser irradiator or a detection sensor by an optical fiber, these can be arranged outside the nozzle. Conventionally, the injection nozzle is heated during aerosol injection for the purpose of preventing clogging of the injection nozzle, but the nozzle can be easily heated by arranging a laser irradiation machine or a sensor outside the nozzle. become able to.

  In the present invention, the laser emitting surface and / or the laser light receiving surface is preferably configured to be flush with the inner peripheral wall surface.

  In this case, since the laser emitting surface and the laser receiving surface are neither depressed nor protruded from the inner peripheral wall surface defining the aerosol flow path, the material particles in the aerosol flow are less likely to adhere to these surfaces. . In addition, nozzle clogging can be prevented.

  Furthermore, the present invention is also a film forming apparatus and a film forming method using the aerosol injection nozzle.

  A film forming apparatus according to the present invention includes: an aerosol generation unit that generates aerosol by dispersing material particles in a carrier gas; and a nozzle that is connected to the aerosol generation unit and sprays the aerosol onto a workpiece. In the membrane device, the nozzle is an aerosol injection nozzle according to the present invention, and further, a physical quantity of a laser beam received by the laser light receiving surface of the nozzle is sensed by the sensor, and based on the sensed physical quantity. A film forming apparatus comprising a calculating means for calculating a particle concentration, a particle size distribution, or a velocity of an aerosol flow passing through the aerosol flow path in the nozzle, wherein the physical quantity is a laser intensity and / or wavelength.

  The film forming method according to the present invention includes an aerosol generating step in which material particles are dispersed in a carrier gas to generate an aerosol, and the generated particles are ejected from a nozzle and sprayed onto an object to be processed to form a film of the material particles. A film forming method including forming a film on a workpiece, wherein the nozzle is an aerosol injection nozzle according to the present invention, and an aerosol flow that passes through the aerosol flow path in the nozzle. On the other hand, an emitting step of emitting a laser from the laser emitting surface of the nozzle, a light receiving step of receiving the laser emitted by the emitting step by the light receiving surface of the nozzle, and a laser received by the light receiving step The sensor detects a physical quantity of the aerosol flow, and based on the sensed physical quantity, the particle concentration of the aerosol flow It includes a calculation step of calculating a particle size distribution or speed, wherein the physical quantity is the intensity and / or wavelength of the laser, a film forming method.

  According to the aerosol injection nozzle, film forming apparatus and film forming method of the present invention, it is possible to accurately measure the particle size distribution, particle velocity, or particle concentration of the aerosol flow in the aerosol deposition method. It becomes.

  Embodiments of the present invention will be specifically described below with reference to the drawings.

  FIG. 1 is a view showing the shape of an aerosol injection nozzle (hereinafter referred to as “injection nozzle”) 21 according to an embodiment of the present invention in front, upper, side, lower and longitudinal sections. However, in these drawings, description regarding the optical fiber of the injection nozzle 21 is omitted. The injection nozzle 21 is composed of a nozzle body 21a, and has a slit-like introduction opening 21f for introducing aerosol into the nozzle at the lower (upstream) end of the nozzle body 21a, and at the upper (downstream) end. , Has a slit-like injection opening 21e for injecting the aerosol to the outside of the nozzle. Further, an aerosol flow path 21b is provided in the nozzle body 21a as a cavity connecting the slit-shaped introduction opening 21f and the slit-shaped injection opening 21e for allowing the aerosol to pass therethrough. Examples of the material constituting the nozzle body 21a include metals and ceramics.

  The shape of the slit-shaped injection opening 21e is a rectangle having a short side of 1 mm or less (for example, about 0.6 to 0.8 mm) and a long side of about 10 to 15 cm as shown in the top view. The shape of the slit-shaped introduction opening 21f is a rectangle having a short side of about 1 cm and a long side of about 10 to 15 cm as shown in the bottom view. That is, the short side of the slit-shaped injection opening 21e is smaller than the short side of the slit-shaped introduction opening 21f. The long sides of both openings have the same length.

  The length of the aerosol channel 21b is about 10 cm.

  The aerosol channel 21b is configured such that its cross-sectional area gradually decreases in the direction from the slit-shaped introduction opening 21f to the slit-shaped injection opening 21e. For this purpose, a pair of tapered portions 21d and 21k are provided on the inner peripheral wall surface of the wide side wall among the inner peripheral wall surfaces that define the aerosol flow path 21b. The pair of tapered portions gently incline inward when the aerosol channel 21b is viewed from upstream to downstream so that the cross-sectional area of the aerosol channel 21b is narrowed by reducing the short side of the cross section. Yes. Further, the pair of taper portions are symmetrical with respect to the inclination angle. As shown in the longitudinal sectional view, the presence of the tapered portions 21d and 21k linearly narrows the length of the short side of the slit-shaped introduction opening 21f to the length of the short side of the slit-shaped injection opening 21e. The length of the taper portions 21d and 21k is about 5 cm.

  The taper portions 21d and 21k are not directly connected to the slit-shaped injection opening 21e, but a pair of flat surface portions 21c and 21j are provided between the taper portions 21d and 21k and the slit-shaped injection opening 21e. Yes. The pair of flat portions are parallel to each other so that the cross-sectional area of the aerosol flow path 21b is constant in this basin. The flat portions 21c and 21j are also parallel to the flow direction of the aerosol flow.

  Further, a pair of plane portions parallel to each other are also provided between the tapered portions 21d and 21k and the slit-like introduction opening 21f.

  The aerosol flow enters the aerosol flow path 21b from the slit-shaped introduction opening 21f. However, since the cross-sectional area of the aerosol flow path 21b is reduced by the tapered portions 21d and 21k, the aerosol flow is accelerated in the middle flow area where the tapered portion is provided. By passing through the downstream area where the flat portions 21c and 21j are provided, the jets are ejected from the slit-shaped ejection openings 21e. That is, the aerosol flow is the fastest in the injection nozzle 21 when passing through the downstream area where the flat portions 21c and 21j are provided.

  2 is an enlarged view of the vertical section of the injection nozzle 21 shown in FIG. 1 in the vicinity of the slit-shaped injection opening 21e, conceptually showing the aerosol flow 22, the laser 61, and the diffracted / scattered light 62 and 63. FIG. . FIG. 2 shows an optical fiber constituting the laser emitting surface and an optical fiber constituting the laser receiving surface.

  On the right side wall 21g of the nozzle body 21a, an optical fiber 32 for laser emission and an optical fiber 42 for wavelength detection of diffracted / scattered light with respect to the flow direction of the aerosol flow 22 (the central axis direction of the aerosol flow path) Embedded in an oblique direction. In addition, the embedding location is about the center in the depth direction of the injection nozzle 21 (short side in the side view of FIG. 1). Since the direction of the optical fiber 32 for laser emission is inclined with respect to the flow direction of the aerosol flow 22, the laser 61 emitted through the optical fiber 32 and the aerosol flow 22 cross each other at an angle.

  However, when the optical fiber 42 for detecting the wavelength of diffracted / scattered light is not provided, that is, when the particle concentration and / or particle size distribution of the aerosol is to be measured but the particle velocity is not to be measured, the laser emission The optical fiber 32 need not be provided obliquely with respect to the flow direction of the aerosol flow 22 and may be provided vertically.

  In this embodiment, the laser emitting optical fiber 32 is inserted from the outer wall surface of the right side wall 21g and travels in the right side wall 21g in such a direction as to incline toward the upstream direction of the aerosol flow 22. Then, it reaches the inner wall surface of the right side wall 21g in the right side plane portion 21c, but is cut there, and the optical fiber cross section 31 that is the laser emission surface is exposed in the aerosol flow path 21b. The optical fiber cross section 31 is processed so as to be flush with the flat surface portion 21c without being depressed or protruding.

  Similarly, the wavelength detection optical fiber 42 for diffracted / scattered light is inserted from the outer wall surface of the right side wall 21 g, but this travels in the right side wall 21 g in a direction inclined toward the downstream direction of the aerosol flow 22. And in the plane part 21c upstream from the point where the cross section 31 of the optical fiber 32 is disposed, it reaches the inner wall surface of the right side wall 21g. The optical fiber cross section 41, which is a laser receiving surface, is cut and exposed in the aerosol flow path 21b. However, the cross section is not depressed or protruded with respect to the flat portion 21c and is flush with the flat surface portion 21c. Has been processed.

  Since the cross section 41 of the wavelength detection optical fiber 42 for diffracted / scattered light is located upstream of the cross section 31 of the laser emitting optical fiber 32, speed measurement utilizing the Doppler effect becomes possible. The angle of inclination of the optical fiber 42 for detecting the wavelength of diffracted / scattered light and the position of its cross section 41 are related to the angle of inclination of the optical fiber 32 for emitting diffracted / scattered light laser and the position of its cross section 31. Adjust to be suitable for receiving diffracted / scattered light necessary for speed measurement using the effect.

  On the other hand, optical fibers 52 and 52a for detecting the intensity of diffracted / scattered light are embedded in the left side wall 21h facing the right side wall 21g with the aerosol channel 21b interposed therebetween. All of them are inserted from the outer wall surface of the left side wall 21h, travel in the left side wall 21h, and then reach the inner wall surface of the left side wall 21h in the left side plane portion 21j. The optical fiber cross-sections 51 and 51a, which are the laser receiving surfaces, are then cut and exposed in the aerosol flow path 21b. However, the cross-section is neither depressed nor protruded from the flat portion 21j. It is processed to become.

  The cross section 51 of the optical fiber 52 is arranged in the straight direction of the laser emitted from the cross section 31 of the diffracted / scattered light laser emitting optical fiber 32, and the inclination angle of the optical fiber 52 is the diffraction / light received by the cross section 51. It is approximately the same as the inclination angle of the optical fiber 32 so that the scattered light is efficiently conducted in the optical fiber 52.

  On the other hand, the cross section 51a of the optical fiber 52a is disposed downstream of the position of the cross section 51 in the plane portion 21j. The inclination angle of the optical fiber 52a is determined according to the position of the cross-section 51a so that the diffracted / scattered light received by the cross-section 51a is efficiently conducted in the optical fiber 52a.

  The measurement of the particle size distribution of the aerosol flow 22 requires calculation of the intensity distribution of diffraction / scattered light, and the measurement of particle concentration requires calculation of the total intensity of diffraction / scattered light. It is better to increase the number of laser receiving surfaces in order to perform more accurately. Therefore, although only two optical fibers for detecting the intensity of diffracted / scattered light are arranged in FIG. In this case, you may arrange | position not only to the plane part 21j by the side of the left side wall 21h but also to the plane part 21c by the side of the right side wall 21g.

  FIG. 3 schematically shows a film forming apparatus using the injection nozzle 21 shown in FIGS. This film forming apparatus includes an aerosol generating unit 10 that generates material particles by dispersing material particles in a carrier gas, and a chamber 20 for film forming inside. The aerosol generation unit 10 is configured so that material particles are accommodated therein and a carrier gas can be introduced. One end of an aerosol supply pipe 11 is inserted into the upper part of the aerosol generation unit 10. An injection nozzle 21 is connected to the other end of the aerosol supply pipe 11.

  The material constituting the material particles is not particularly limited as long as it can be used in the aerosol deposition method. For example, lead zirconate titanate (PZT) which is a piezoelectric material, inorganic powder such as alumina, resin Organic powders such as can be used. In this embodiment, ceramics are used as the material constituting the material particles.

  The particle size of the material particles may be any particle size that can be used for the aerosol deposition method, but may be, for example, about several μm to several tens of μm.

  The carrier gas is not particularly limited as long as it can be used in the aerosol deposition method, and for example, inert gas such as helium and argon, nitrogen, air, oxygen and the like can be used.

  Inside the chamber 20, a substrate holder 24 for mounting a substrate 23, which is an object to be processed, and an injection nozzle 21 are disposed below the substrate holder 24. The substrate holder 24 is formed in a rectangular plate shape, and is suspended from the ceiling of the chamber 20 in a horizontal posture by the substrate holder moving mechanism 25 so that the substrate 23 can be held on the lower surface side thereof. The substrate holder moving mechanism 25 can be driven in accordance with a command from the control device, whereby the substrate holder 24 can move in the front-rear direction and the left-right direction in the horizontal plane.

  A booster pump, a rotary pump, or the like is connected to the chamber 20 so that the inside thereof can be decompressed.

  The material of the substrate 23 used in the present invention is not particularly limited, and may be, for example, metal, silicon, semiconductor, resin, or the like.

  The injection nozzle 21 is the same as that shown in FIGS. The slit-shaped introduction opening 21f is connected to the other end of the aerosol supply pipe 11, from which the aerosol is introduced into the nozzle. The slit-shaped injection opening 21e is directed to the surface of the substrate 23 held on the lower surface of the substrate holder 24, on which the ceramic thin film is to be formed, from which the aerosol flow 22 is ejected. In FIG. 3, the injection nozzle 21 is arranged in such a direction as to inject the aerosol flow 22 perpendicularly to the substrate 23, but may be arranged in a direction to inject obliquely with respect to the substrate 23. .

  As described above, the optical fiber cross-section 31 that is the laser emission surface, the optical fiber cross-section 41 that is the laser light receiving surface for wavelength detection, and the laser light reception for intensity detection are provided on the inner peripheral wall surface that defines the aerosol flow path 21b in the injection nozzle 21. Optical fiber cross sections 51 and 51a are provided. The optical fiber cross section 31 is connected to a laser irradiator 33 by an optical fiber 32. The optical fiber cross section 41 is connected to an optical wavelength detection sensor 43 by an optical fiber 42, and the sensor is further connected to a speed calculation unit 44. The optical fiber cross sections 51 and 51a are connected to light intensity detection sensors 53 and 53a by optical fibers 52 and 52a, and the sensors are further connected to a particle size distribution and / or particle concentration calculation unit 54.

  In the aerosol generation unit 10, an ultrasonic vibration device is arranged to apply vibration, a hoisting gas is introduced into the cyclone flow to generate a cyclone flow, or a flowing gas is supplied from the floor portion to thereby generate a carrier gas. The material particles are dispersed in the aerosol to generate aerosol. Here, when the internal pressure of the chamber 20 is made lower than the internal pressure of the aerosol generating unit 10, the aerosol in the aerosol generating unit 10 is sucked into the aerosol supply pipe 11 due to the differential pressure, and injected through this. It is supplied to the nozzle 21. In the middle of the aerosol supply pipe 11, a gas replenishing pipe for replenishing the carrier gas may be connected so that the total amount of the carrier gas can be adjusted.

  The aerosol that has entered the aerosol flow path 21b from the slit-shaped introduction opening 21f is accelerated because the cross-sectional area is reduced by the taper portions 21d and 21k in the midstream area of the flow path, and further, the plane portions 21c and 21j It passes through the provided downstream area, and is ejected to the outside of the ejection nozzle 21 from the slit-shaped ejection opening 21 e and sprayed onto the substrate 23. When passing through the downstream area where the flat portions 21c and 21j are provided, the aerosol flow becomes the fastest and the flow direction is parallel to the flat portions 21c and 21j. Particle adhesion to the optical fiber cross-sections 31, 41, 51, 51a is suppressed. This is because the flow direction is parallel to the flat portions 21c and 21j, so that there are few opportunities for particles to contact the flat portions 21c and 21j, and the flat portion 21c temporarily due to moisture or the like adhering to the powder. , 21j even if it adheres to the adhering powder, the rapidly flowing powder collides with the adhering powder and peels off from the flat portions 21c, 21j. Then, the material particles colliding with the surface of the substrate 23 are crushed and deposited to form a ceramic thin film. A ceramic thin film can be formed on the entire surface of the substrate 23 by moving the substrate holder 24 little by little in the horizontal plane when spraying the aerosol flow 22. A ceramic thin film having an arbitrary shape may be formed at an arbitrary position on the substrate 23 by installing a mask having a predetermined pattern between the slit-shaped injection opening 21 e and the substrate 23.

  The laser for measuring the particle velocity, the particle size distribution, and / or the particle concentration is generated by the light emitted from the laser irradiator 33, transmitted by the optical fiber 32, and emitted from the optical fiber cross section 31 into the aerosol flow path 21b. The emitted laser 61 irradiates the aerosol flow 22 passing through the downstream area where the flat portions 21c and 21j are located immediately before being ejected from the slit-shaped ejection opening 21e. The diffracted / scattered light generated by the laser 61 being diffracted and scattered by the aerosol flow 22 is produced by the optical fiber cross section 41 on the wall surface where the laser is emitted and on the wall surface facing the wall surface. , 51a.

  The diffracted / scattered light received by the optical fiber cross section 41 is transmitted to the optical wavelength detection sensor 43 by the optical fiber 42, where the wavelength is detected. The output of the detected wavelength is transmitted to the velocity calculation unit 44, where it is digitized by an A-D converter, and then the particle velocity is calculated based on the detected wavelength.

  On the other hand, the diffracted / scattered light received by the optical fiber cross sections 51 and 51a is transmitted to the light intensity detection sensors 53 and 53a by the optical fibers 52 and 52a, and the light intensity is detected there. The detected intensity output is transmitted to the particle size distribution and / or particle concentration calculation unit 54, where it is digitized by an A-D converter, and then an intensity pattern and total intensity are obtained. The particle size distribution and particle concentration are calculated.

  In the present invention, since the particle velocity, particle concentration, and particle size distribution of the aerosol flow 22 can be calculated in real time, the measured particle velocity, particle concentration can be obtained even during the aerosol deposition method. The result of the particle size distribution is fed back to the conditions for generating aerosol in the aerosol generating unit 10, the amount of gas supplemented by the gas supplementing pipe, the condition for spraying the aerosol flow 22 on the substrate, etc. By adjusting the thickness, the thickness of the formed ceramic thin film can be made uniform, and the quality can be improved. Further, when an abnormality occurs in the particle velocity or the like of the aerosol flow 22 measured in real time, it is possible to immediately stop the production and prevent any defects from occurring in the product in advance.

  As described above, the present invention is not limited to the form in which the optical fiber embedded in the injection nozzle and the laser irradiation machine, the light wavelength detection sensor, or the light intensity detection sensor are connected. The head, the head of the optical wavelength detection sensor, or the head of the light intensity detection sensor may be provided directly on the inner peripheral wall surface of the aerosol flow path.

The figure which showed the shape of the aerosol injection nozzle which concerns on one Embodiment of this invention with the front, the upper surface, the side surface, the lower surface, and the longitudinal cross-section. The figure which expanded the longitudinal cross section of slit-shaped injection opening 21e vicinity about the aerosol injection nozzle shown in FIG. 1, and showed conceptually with the aerosol flow, the laser, and the diffracted / scattered light. Schematic showing a film forming apparatus using the aerosol injection nozzle shown in FIG. 1 and FIG.

Explanation of symbols

DESCRIPTION OF SYMBOLS 10 Aerosol generating part 11 Aerosol supply pipe | tube 20 Chamber 21 Injection nozzle 21a Nozzle main body 21b Aerosol flow path 21c, 21j Plane part 21d, 21k Taper part 21e Slit-like injection opening 21f Slit-like introduction opening 21g Right side wall 21h Left side wall 22 Aerosol flow 23 Substrate 24 Substrate holder 25 Substrate holder moving mechanism 31 Cross section of optical fiber 32 Optical fiber for laser emission 33 Laser irradiator 41 Cross section of optical fiber 42 Optical fiber for wavelength detection of diffracted / scattered light 43 Optical wavelength detection sensor 44 Speed calculation Sections 51 and 51a Cross sections 52 and 52a of optical fibers 52 and 52a Optical fibers 53 and 53a for detecting the intensity of diffracted / scattered light Light intensity sensor 54 Particle size distribution and / or particle concentration calculation section 61 Lasers 62 and 63 Diffraction / scattering light

Claims (8)

An aerosol injection nozzle comprising an introduction opening for introducing aerosol, an injection opening for injecting aerosol, and an aerosol flow path for allowing aerosol to pass from the introduction opening to the injection opening,
The inner peripheral wall surface defining the aerosol flow path is provided with a laser emitting surface and a laser receiving surface,
The laser emitting surface is a surface for emitting a laser of a laser irradiation device, from which laser is emitted into the aerosol flow path,
An aerosol injection nozzle, wherein the laser light receiving surface is a light receiving surface of a sensor that detects a physical quantity of a laser and receives a laser emitted from the laser emitting surface. A part of the inner peripheral wall surface is a tapered portion formed so as to reduce the cross-sectional area of the aerosol flow path as it goes downstream;
The aerosol injection nozzle according to claim 1, wherein the laser emitting surface and the laser receiving surface are provided in a portion of the inner peripheral wall surface downstream of the tapered portion. The inner peripheral wall surface includes a pair of parallel flat portions facing each other across the central axis of the aerosol flow path,
The nozzle for aerosol injection according to claim 1 or 2, wherein the laser emitting surface and the laser receiving surface are provided on the flat portion.   The nozzle for aerosol injection according to any one of claims 1 to 3, wherein a laser is emitted from the laser emission surface in an oblique direction with respect to a central axis of the aerosol flow path.   The nozzle for aerosol injection according to any one of claims 1 to 4, wherein the laser emitting surface and / or the laser receiving surface is constituted by a cross section of an optical fiber.   The nozzle for aerosol injection according to any one of claims 1 to 5, wherein the laser emitting surface and / or the laser light receiving surface is configured to be flush with the inner peripheral wall surface. An aerosol generation unit that generates aerosol by dispersing material particles in a carrier gas, and a nozzle that is connected to the aerosol generation unit and sprays the aerosol onto an object to be processed,
The nozzle is an aerosol injection nozzle according to any one of claims 1 to 6,
Further, the physical quantity of the laser beam received by the laser light receiving surface of the nozzle is sensed by the sensor, and based on the sensed physical quantity, the particle concentration, the particle size distribution of the aerosol flow passing through the aerosol flow path in the nozzle, or A calculating means for calculating the speed;
A film forming apparatus, wherein the physical quantity is a laser intensity and / or wavelength. An aerosol generating step of dispersing material particles in a carrier gas to generate an aerosol, and forming a film of the material particles on the object to be processed by ejecting the generated aerosol from a nozzle and spraying it on the object to be processed A film forming method comprising:
The nozzle is an aerosol injection nozzle according to any one of claims 1 to 6,
Further, for the aerosol flow passing through the aerosol flow path in the nozzle, an emitting step of emitting a laser from the laser emitting surface of the nozzle;
A light receiving step of receiving the laser emitted by the emitting step by the light receiving surface of the nozzle;
Detecting a physical quantity of the laser beam received by the light receiving process with the sensor, and calculating a particle concentration, a particle size distribution or a velocity of the aerosol flow based on the sensed physical quantity, and
The film forming method, wherein the physical quantity is laser intensity and / or wavelength.

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