JP2008240017A - Vacuum vapor deposition apparatus - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a vacuum vapor deposition apparatus with which one or two of a plurality of mutually different kinds of vapor deposition sources each holding an organic compound can be simultaneously opened and mutual contamination between the plurality of mutually different kinds of vapor deposition sources can be prevented. <P>SOLUTION: In the vacuum vapor deposition apparatus 100, three vapor deposition sources 120, 130, 140 holding mutually different kinds of organic vapor deposition materials 121, 131, 141, respectively, are arranged on the bottom face wall of a vacuum chamber 110 at an arrangement angle θ being nearly equal angle with respect to the rotation center O of a rotation shaft 181 for rotating a shutter 180, and then a thin film comprising organic compounds is deposited on a substrate held with a substrate holder by rotating the shutter 180 by an angle unit that is 1/2 times of the arrangement angle θ of the vapor deposition sources 120, 130, 140 to open one of or to simultaneously open two of the three vapor deposition sources 120, 130, 140 and at the same time, to shield the other vapor deposition sources except for the opened deposition source. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to a vacuum deposition apparatus for forming a thin film of an organic compound on a substrate.

  2. Description of the Related Art Conventionally, there is known a vacuum evaporation apparatus that forms a thin film (film formation) by evaporating an evaporation material from an evaporation source in a vacuum atmosphere and attaching the vapor to the surface of an object to be evaporated. For example, in the field of manufacturing optical articles, for example, an antireflection film, an antifouling film having antifouling performance, or an antifogging functional film having antifogging performance is formed on a glass substrate by using this vacuum deposition apparatus. It is used to do.

In recent years, the types of vapor deposition materials used for vapor deposition sources have increased, and the optimum film formation conditions differ for each material type. In order to cope with such film formation, a plurality of vapor deposition sources (usually two types) are arranged in the same vapor deposition apparatus, and film formation is performed by switching the vapor deposition source according to the substance used (for example, Patent Documents). 1).
In addition, a functional organic coating that imparts water repellency, oil repellency, etc., generally formed using a wet method such as an immersion method, is replaced with a vacuum deposition method instead of the wet method for the purpose of improving workability. There has been proposed a surface treatment method for forming a film by using (see, for example, Patent Document 2).

Japanese Patent Laid-Open No. 11-124667 JP-A-5-239243

  When using a vapor deposition apparatus such as that disclosed in Patent Document 1 to switch between two types of vapor deposition sources (vapor deposition materials), a shutter provided for each vapor deposition source is operated, and one of the substances is While the seed is being deposited, the vapor adheres to the surface around the deposition source including the other heating means. When switching to the other evaporation substance, another substance attached to the periphery of the evaporation source including the heating means is also evaporated, and the purity of the film substance to be formed is inferior. In particular, in the case of depositing an organic material as disclosed in Patent Document 2, it is often deposited under a relatively low vacuum condition as compared to an inorganic material, and the vapor of the organic material is easily diffused to the periphery, and two deposition sources Even if a shielding plate or the like is provided between them, it is difficult to prevent the evaporation source including the heating means from being contaminated.

  In addition, since the conventional vapor deposition apparatus can use only one vapor deposition source in one vapor deposition, when forming a mixed film composed of two or more kinds of materials, these materials are previously stored in one vapor deposition source. Used mixed. For this reason, a chemical reaction occurs in the mixed substance and it is easy to change to another substance, and it is difficult to form a desired mixed film.

  Therefore, the present invention has been made in view of such circumstances, and enables one or two of a plurality of different types of vapor deposition sources holding organic compounds to be simultaneously opened. Another object of the present invention is to provide a vacuum vapor deposition apparatus that prevents the occurrence of contamination among a plurality of vapor deposition sources.

  In order to solve the above problems, a vacuum vapor deposition apparatus of the present invention is a vacuum vapor deposition apparatus for forming a thin film made of an organic compound on a substrate by vapor deposition, and the vacuum chamber and the vacuum chamber are of the same type. A plurality of vapor deposition sources individually holding the different organic compounds, and between the plurality of vapor deposition sources and the substrate, the vapors of the organic compounds held in the plurality of vapor deposition sources are opened and shielded The shutter has an open region that simultaneously opens two of the plurality of vapor deposition sources, and rotates around the center of the vacuum chamber as a rotation axis.

  According to this configuration, a vacuum vapor deposition apparatus for forming a thin film made of an organic compound on a substrate by vapor deposition includes a plurality of vapor deposition sources that individually hold different types of organic compounds in a vacuum chamber, and a plurality of vapor deposition sources. One shutter for opening and shielding the vapor of the organic compound held in the plurality of deposition sources is provided between the plurality of deposition sources and the substrate, and the shutter includes two shutters of the plurality of deposition sources. It is possible to deposit two types of organic compounds of two different types at the same time by rotating around the rotation axis. Therefore, a mixed film of organic compounds that causes a chemical reaction by mixing two kinds of compositions can be formed with high purity. In addition, since a plurality of vapor deposition sources for holding different types of organic compounds are provided, a mixed film made of a desired organic compound can be continuously formed in multiple layers.

  Further, in the vacuum vapor deposition apparatus of the present invention, the plurality of vapor deposition sources are arranged at an arrangement angle substantially equal to the rotation center of the shutter, and the shutter rotates about the rotation axis, It is preferable that the open region simultaneously opens one or two of the plurality of vapor deposition sources and shields the other vapor deposition sources other than the opened vapor deposition sources.

  According to this configuration, the plurality of vapor deposition sources that hold different types of organic compounds disposed in the vacuum chamber of the vacuum vapor deposition apparatus are arranged at substantially equal angular angles with respect to the rotation center of the shutter. The shutter is rotated about the rotation axis, and the open region simultaneously opens one or two of the plurality of deposition sources and shields other deposition sources except the opened deposition source. As a result, it is possible to simultaneously deposit one organic compound or two selected organic vapor deposition materials among a plurality of selected vapor deposition sources. Therefore, the vapor deposition film of the selected organic compound and the mixed film made of the two selected organic vapor deposition materials can be continuously formed. In addition, the shutter shields one of the plurality of vapor deposition sources or other vapor deposition sources other than the vapor deposition sources that are simultaneously opened, so that the shutter is easily released from the open vapor deposition source and diffuses to the periphery. It is possible to prevent organic compound vapor from adhering to and contaminating other deposition sources, and to prevent shielded vapor deposition of other deposition sources from being contaminated between multiple deposition sources. .

In the vacuum vapor deposition apparatus of the present invention, it is preferable that the shutter can be rotated every ½ angle unit of the arrangement angle where the plurality of vapor deposition sources are arranged.
According to this configuration, the shutter is 1/2 (half) of the deposition angle of the deposition source with respect to the plurality of deposition sources disposed at substantially the same angle with respect to the rotation center of the shutter. By being rotatable for each angular unit, one of a plurality of vapor deposition sources or a combination of two vapor deposition sources that are simultaneously opened can be arbitrarily selected.

  Also, the vacuum deposition apparatus of the present invention is characterized in that, among the plurality of deposition sources, at least two of the organic compounds held by the deposition source opened simultaneously by the shutter have different boiling points. It is preferable to do.

  According to this configuration, since the boiling points of different kinds of organic compounds held in the vapor deposition source in which at least two of the vapor deposition sources are simultaneously opened by the shutter are close to each other, When forming a mixed film of organic compounds, even if different organic compound substances adhere to each other's vapor deposition source, they are not deposited because they are heated to a temperature at which each organic compound evaporates. . In addition, when the boiling points of the organic compounds held in the vapor deposition sources other than the two vapor deposition sources that are simultaneously opened are close to each other, the multi-layer is continuously formed while maintaining the vacuum state in the vacuum chamber. An organic film can be formed, and the working efficiency of the vapor deposition process is improved. In addition, as for the range where a boiling point adjoins, the difference of a mutual boiling point is 100 degrees C or less.

  DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments relating to a vacuum deposition apparatus of the present invention will be described below with reference to the drawings.

  FIG. 1 is a side sectional view showing an outline of the vacuum vapor deposition apparatus of the present invention, and FIG. 2 is a sectional view taken along line AA of the vacuum vapor deposition apparatus shown in FIG. In addition, the part shown by an arrow along the AA line of FIG. 1 shows sectional drawing in the BOB line shown in FIG.

  1 and 2, the vacuum vapor deposition apparatus 100 includes a first vapor deposition source 120, a second vapor deposition source 130, a third vapor deposition source 140, and deposition vessels 150, 160, and 170 in a vacuum chamber 110. A shutter 180 and a substrate holder 190 for holding a large number of substrates 10 to be deposited are provided.

  The first vapor deposition source 120, the second vapor deposition source 130, and the third vapor deposition source 140 are provided on the bottom wall side in the vacuum chamber 110, and the substrate holder 190 is provided on the ceiling side. The shutter 180 is disposed between the first vapor deposition source 120, the second vapor deposition source 130, the third vapor deposition source 140, and the substrate holder 190.

  The vacuum chamber 110 is provided with an exhaust port 111 on the side wall. The exhaust port 111 is connected to a vacuum pump that is a combination of a dry pump and a turbo molecular pump (not shown). A predetermined vacuum state is secured by evacuating the vacuum chamber 110 by operating the vacuum pump. The vacuum pump is connected to a control unit (not shown) and controlled by this control unit.

  The first vapor deposition source 120, the second vapor deposition source 130, and the third vapor deposition source 140 are resistance heating vapor deposition sources, and all have the same structure. Hereinafter, the first vapor deposition source 120, the second vapor deposition source 130, and the third vapor deposition source 140 may be expressed as the vapor deposition source 120, the vapor deposition source 130, and the vapor deposition source 140.

  In the vapor deposition sources 120, 130, and 140, an organic vapor deposition material as an organic compound for vapor deposition is placed and held in a boat-type container made of a filament material such as tungsten, tantalum, and molybdenum. The vapor deposition source 120 holds a first organic vapor deposition material 121, the vapor deposition source 130 holds a second organic vapor deposition material 131, and the vapor deposition source 140 holds a third organic vapor deposition material 141. Hereinafter, the first organic vapor deposition material 121, the second organic vapor deposition material 131, and the third organic vapor deposition material 141 may be expressed as the organic vapor deposition material 121, the organic vapor deposition material 131, and the organic vapor deposition material 141.

The vapor deposition sources 120, 130, and 140 are heated by generating resistance heat when a current is supplied from a power source (not shown) to a boat type container in which each organic vapor deposition material is held, and held in each boat type container. The deposited organic vapor deposition materials 121, 131, 141 are heated. That is, the boat-type container functions as a heating unit that heats the organic vapor deposition material held in the container.
The first vapor deposition source 120, the second vapor deposition source 130, and the third vapor deposition source 140 configured as described above are housed and held in the deposition preventing containers 150, 160, and 170, respectively.

  The anti-adhesion containers 150, 160, and 170 are containers having the same structure and made of, for example, stainless steel, and have openings 151, 161, and 171 that open toward the ceiling of the vacuum chamber 110. The deposition containers 150, 160, and 170 are used when vapors of the organic deposition materials 121, 131, and 141 held in the boat-type containers of the three deposition sources 120, 130, and 140 are deposited on the substrate 10. The organic evaporating substances released from the respective vapor deposition sources 120, 130, and 140 have a function of preventing each other from adhering to and contaminating the vapor deposition sources.

  In addition, 150, 160, and 170 in which the vapor deposition sources 120, 130, and 140 are accommodated are rotated on the bottom wall of the vacuum chamber 110 at a position equidistant from the rotation center O of the rotation shaft 181 of the shutter 180 described later. The shafts 181 are arranged at the same arrangement angle θ around the rotation center O (see FIG. 2). That is, the arrangement angle θ in the present embodiment is 120 °.

The shutter 180 is fixed to the rotary shaft 181 and is rotatably supported at the center of the bottom wall of the vacuum chamber 110.
The rotation shaft 181 extends outside through the bottom wall of the vacuum chamber 110, and a motor 182 for driving the rotation shaft 181 to rotate is connected to the end. That is, the motor 182 rotates the shutter 180.

  The shutter 180 is at least one of the openings 151, 161, 171 of the deposition containers 150, 160, 170 in which the first deposition source 120, the second deposition source 130, and the third deposition source 140 are accommodated. The opening has a size capable of covering two openings at the same time, and is disposed adjacent to the openings 151, 161, 171 of the deposition preventing containers 150, 160, 170. The specific shape of the shutter 180 will be described later with reference to FIG.

  A smaller vertical distance α (see FIG. 1) between the upper portions (openings 151, 161, 171) of the deposition-proof containers 150, 160, 170 and the shutter 180 is preferable, but a reliable operation of the shutter 180 is ensured. In addition, in order to prevent the vapor emitted from the respective vapor deposition sources 120, 130, and 140 from flowing in, a range of about 1 mm to 5 mm is preferable.

  An encoder (not shown) for detecting the rotation position of the motor 182 (that is, the position of the rotation shaft 181 and the shutter 180) is attached to the motor 182 that rotationally drives the rotation shaft 181. Based on this, the motor 182 is rotationally controlled. The motor 182 and the encoder are connected to a control unit (not shown) and controlled by the control unit. When the motor 182 is driven to rotate, the rotating shaft 181 rotates, and the shutter 180 fixed to the rotating shaft 181 rotates around the rotating shaft 181 as a rotation center.

  The substrate holder 190 is a holder formed in a dome shape, and a large number of openings are formed, and the substrate 10 on which a thin film made of each organic vapor deposition material is deposited is held in the many openings. Further, the substrate holder 190 is configured such that the central portion of the dome-shaped upper surface is detachable from the holder rotation shaft 191, and is held and fixed to the holder rotation shaft 191 that is rotatably supported by the central portion of the ceiling wall of the vacuum chamber 110. Yes. Accordingly, the substrate holder 190 is disposed toward the openings 151, 161, 171 of the deposition containers 150, 160, 170, that is, the first deposition source 120, the second deposition source 130, and the third deposition source 140. ing.

  One end of the holder rotating shaft 191 on which the substrate holder 190 is held and fixed extends through the ceiling wall of the vacuum chamber 110 and extends to the outside. In order to average the film thickness between the substrates 10 on which the vapor deposition material is deposited, a holder rotating motor 192 that rotates the holder rotating shaft 191 (that is, the substrate holder 190) is connected.

Next, the outer shape of the shutter 180 will be described.
FIG. 3 is a cross-sectional view of the vacuum evaporation apparatus as viewed from the bottom direction of the vacuum chamber. Note that the shutter 180 shown in FIG. 3 shows a mode in which two of the three vapor deposition sources 120, 130, and 140 are shielded and the vapor deposition source 140 is opened.

  In FIG. 3, the shutter 180 is an area DA (shown by hatching in FIG. 3) that covers the opening 151 of the deposition preventing container 150 in which the deposition source 120 is accommodated among the three deposition sources 120, 130, and 140. A region DC (shown by hatching in FIG. 3) covering the opening 161 of the deposition preventing container 160 in which one of the vapor deposition sources 130 and 140 adjacent to the vapor deposition source 120 is accommodated, and the vapor deposition source A region DB (shown by hatching in FIG. 3) indicated by a two-dot chain line at a position where the opening 151 of the deposition preventing container 150 in which 120 is accommodated is rotated 180 ° about the rotation center O of the rotation shaft 181. It is formed including.

  At least the area other than the area DA, the area DB, and the area DC is an open area that allows two of the plurality of vapor deposition sources to be simultaneously opened. This open area can open one or two of the plurality of vapor deposition sources at the same time.

The outer shape of the shutter 180 will be specifically described.
The shutter 180 has a center connecting a semicircle with a radius γ centered on the rotation center O of the rotation shaft 181 and the center of the rotation shaft 181 and the center of the opening 151 of the deposition preventing container 150 in which the vapor deposition source 120 is accommodated. An outer shape surrounded by a width line that is separated from the line by a dimension γ in both directions and a line that is orthogonal to the width line that is positioned closer to the outer peripheral wall of the vacuum chamber 110 than the opening 151 of the deposition preventing container 150 (FIG. 3). Δ, which is indicated by hatching with a wide interval in between, and the outer shape δ are connected to the outermost shape in the shape rotated right by 120 ° and 180 ° with the rotation shaft 181 as the rotation center.

  The dimension γ is set in a range that includes at least the opening 151 of the deposition preventing container 150 and does not reach the opening 171 of the deposition preventing container 170 in which the vapor deposition source 140 is accommodated. Further, the shape (position) in the outer peripheral direction of the outer shape δ can be set in a range including at least the opening 151 of the deposition preventing container 150 and not reaching the vacuum chamber 110. Therefore, the outer shape of the shutter 180 may be any shape as long as these conditions are satisfied.

The shutter 180 having such an outer shape is configured to be rotatable for each angle unit (rotation angle unit) β along with the rotation of the rotation shaft 181 by the rotation of the motor 182.
The rotation of the shutter 180 for each rotation angle unit β is controlled by the control signal of the control unit based on the detection position of the encoder by the motor 182.

  The rotation angle unit β is 1/2 (with respect to the disposition angle θ in which the vapor deposition sources 120, 130, and 140 are disposed at the same disposition angle θ (120 °) around the rotation center O of the rotation shaft 181. Half) is 60 °. The stop position of the shutter 180 at a predetermined rotational angle unit is the position a of the center line connecting the center of the rotating shaft 181 and the center of the opening 151 of the deposition preventing container 150 in which the vapor deposition source 120 is accommodated. The base line can be stopped at six base line positions from position a to position f for each rotation angle unit β (60 °) from the base line.

Next, the operation of the shutter 180 will be described.
FIG. 4 is a cross-sectional view of the vacuum deposition apparatus as viewed from the bottom direction of the vacuum chamber showing the mode at the stop position for each rotation angle unit β (60 °) of the shutter, and illustrates the mode for each rotation angle unit in order. 4 (a) to 4 (f).

  4A, the center line of the outer shape δ (see FIG. 3) of the shutter 180 is positioned at the position a (the rotation center O of the rotating shaft 181 and the opening 151 of the deposition preventing container 150 in which the vapor deposition source 120 is accommodated. The center line is connected to the center of FIG. 4B, and the stopped state is shown in FIG. 4B. Moreover, the state stopped to the position c-the position f is shown in FIG.4 (c)-FIG.4 (f) in order.

  4A, when the center line of the outer shape δ part of the shutter 180 (hereinafter referred to as a predetermined position) is stopped at the position a, the opening 151 (first deposition source) of the deposition preventing container 150 is used. 120), and the opening 161 (second deposition source 130) of the deposition preventing container 160 is shielded, and the opening 171 (third deposition source 140) of the deposition preventing container 170 is open.

  In FIG. 4B, when the predetermined position of the shutter 180 is stopped at the position b, the opening 171 (third deposition source 140) of the deposition preventing container 170 is shielded and the opening of the deposition preventing container 150 is opened. 151 (first vapor deposition source 120) and the opening 161 (second vapor deposition source 130) of the deposition preventing container 160 are in an open state.

  In FIG. 4C, when the predetermined position of the shutter 180 is stopped at the position c, the opening 161 (second vapor deposition source 130) of the deposition preventing container 160 and the opening 171 (first) of the deposition preventing container 170 are displayed. 3 deposition source 140) is shielded, and the opening 151 (first deposition source 120) of the deposition preventing container 150 is open.

  In FIG. 4D, when the predetermined position of the shutter 180 is stopped at the position d, the opening 151 (first vapor deposition source 120) of the deposition preventing container 150 is shielded, and the opening 161 of the deposition preventing container 160 is shielded. (Second vapor deposition source 130) and opening 171 (third vapor deposition source 140) of deposition preventing container 170 are in an open state.

  In FIG. 4 (e), when the predetermined position of the shutter 180 is stopped at the position e, the opening 151 (first vapor deposition source 120) of the deposition preventing container 150 and the opening 171 (third) of the deposition preventing container 170 are displayed. The deposition source 140) is shielded, and the opening 161 (second deposition source 130) of the deposition preventing container 160 is in an open state.

  In FIG. 4 (f), when the predetermined position of the shutter 180 is stopped at the position f, the opening 161 (second vapor deposition source 130) of the deposition preventing container 160 is shielded, and the opening 151 of the deposition preventing container 150. (First vapor deposition source 120) and opening 171 (third vapor deposition source 140) of deposition preventing container 170 are in an open state.

  As described above, the shutter 180 is stopped at the position a to the position f every rotation angle unit 60 °, thereby simultaneously shielding one or two of the three vapor deposition sources 120, 130, and 140. Other deposition sources except the shielded deposition source can be opened. That is, the organic vapor deposition materials 121, 131, and 141 held in the boat-type containers of the three vapor deposition sources 120, 130, and 140 are opened singly or in combination, and the organic vapor deposition materials are removed from the substrate 10. Can be deposited on top. Moreover, the combination of the organic vapor deposition material which vapor-deposits two simultaneously can be selected arbitrarily.

  In particular, it is possible to deposit two different organic vapor deposition materials at the same time, thereby forming a mixed film of organic vapor deposition materials that cause a chemical reaction by mixing two types of compositions in advance. This is effective when Of course, thin films of three different types of organic vapor deposition materials 121, 131, and 141 can also be successively formed in a predetermined order.

  Note that the position a to the position f where the predetermined position of the shutter 180 stops, that is, the selection and combination of the organic vapor deposition materials 121, 131, 141 to be vapor deposited are controlled by the motor 182 being rotated based on the control signal of the control unit. , Can be arbitrarily selected (set).

  Using the vacuum vapor deposition apparatus 100 configured as described above, a thin film of the first organic vapor deposition material 121, the second organic vapor deposition material 131, and the third organic vapor deposition material 141 as an organic compound on the surface of the substrate 10 ( An example of vapor deposition for forming an organic thin film will be described.

  As the substrate 10 on which the organic thin film is formed, an optical article such as a spectacle lens, a lens and a hybrid lens for optical equipment, a mirror, a cover glass for a wristwatch, a display board for a mobile phone, a cover for various displays, Recording media such as CD (Compact Disc), and other optical elements such as a lens array and a prism. The material of the substrate 10 is not particularly limited, and may be glass or plastic. However, when the material of the substrate 10 is plastic, an inorganic material layer is preferably formed below the organic film to be formed.

(Vapor deposition example 1)
Vapor deposition example 1 is a vapor deposition example in which a glass lens is used as the substrate 10 and three types of antifogging organic films of different types are formed on the glass lens. Hereinafter, in the vapor deposition example 1, the glass lens is referred to as a glass lens 10 instead of the substrate 10.
The antifogging organic film formed on the glass lens 10 has a function of imparting antifogging performance by forming a hydrophobic functional film on the surface of the glass lens 10.

  The first organic vapor deposition material 121 used to form the antifogging organic film is an amino group-containing coupling agent 4-aminobutyltrimethoxyxylan, and the second organic vapor deposition material 131 has an amino group at the end. As the surface active silicon 6-aminohexyltrimethoxysilane and the third organic vapor deposition material 141, nonionic surfactant polyoxyethylene nonylphenyl ether was prepared.

  The antifogging organic film formed on the glass lens 10 using these organic vapor deposition materials 121, 131, 141 is composed of a first organic vapor deposition material 121 (4-aminobutyltrimethoxyxylan) and a third organic vapor deposition material. After the vapor deposition material (polyoxyethylene nonylphenyl ether) is vapor deposited at the same time to form the first mixed film, the second organic vapor deposition material 131 (6-aminohexyltrimethoxysilane) is formed on the first mixed film. And a third organic vapor deposition material (polyoxyethylene nonylphenyl ether) are vapor-deposited simultaneously to form a second mixed film.

  This is because polyoxyethylene nonylphenyl ether (third organic vapor deposition material 141) is preliminarily made of 4-aminobutyltrimethoxyxysilane (first organic vapor deposition material 121) or 6-aminohexyltrimethoxysilane (second organic vapor deposition material 141). When mixed with the vapor deposition material 131), a chemical reaction is easily caused to change to another substance, and thus an antifogging organic film is formed by such a vapor deposition method. The boiling points of these organic vapor deposition materials 121, 131, and 141 are all about 250 ° C. Note that 4-aminobutyltriethoxysilane can be used as the first organic vapor deposition material 121, and 6-aminohexyltriethoxysilane can be used as the second organic vapor deposition material 131. When mixed with nonylphenyl ether, a chemical reaction is caused to easily change to another substance.

In the vacuum vapor deposition method on the glass lens 10 using these organic vapor deposition materials 121, 131, 141, first, the glass lens is formed in a large number of openings of the substrate holder 190 removed from the holder rotating shaft 191 of the vacuum vapor deposition apparatus 100. 10 is placed.
Then, the substrate holder 190 on which the glass lens 10 is placed is attached to the holder rotation shaft 191 in the vacuum chamber 110.

  On the other hand, the first organic vapor deposition material 121 is charged and held in the first vapor deposition source 120 (boat-type container). Similarly, the second organic vapor deposition material 131 is held in the second vapor deposition source 130, and the third organic vapor deposition material 141 is held in the third vapor deposition source 140.

After the organic vapor deposition material 121, the organic vapor deposition material 131, and the organic vapor deposition material 141 are held in the respective vapor deposition sources (boat-type containers), the motor 182 operates to rotate the shutter 180 along with the rotation of the rotating shaft 181. The shutter 180 is rotated to a position f at a predetermined position of the shutter 180 (center line of the outer shape δ portion, see FIG. 3), and stops at the position f (see FIG. 4 (f)).
Thereby, the vapor deposition source 120 holding the organic vapor deposition material 121 and the vapor deposition source 140 holding the organic vapor deposition material 141 are opened, and the vapor deposition source 130 holding the organic vapor deposition material 131 is blocked.

Then, a vacuum pump combining a dry pump and a turbo molecular pump is operated, and the inside of the vacuum chamber 110 is exhausted to an ultimate pressure of about 1 × 10 ⁻² Pa through an exhaust port 111 formed on the side wall of the vacuum chamber 110. The

  Then, the holder rotating motor 192 is driven to rotate the substrate holder 190 on which a large number of glass lenses 10 are placed, and current is supplied to the vapor deposition sources 120, 130, and 140 to resist the boat-type container. Heat is generated, and the organic vapor deposition materials 121, 131, 141 held in the vapor deposition sources 120, 130, 140 are heated. The temperatures at which the organic vapor deposition materials 121, 131, and 141 are heated are all about 300 ° C.

  Thereby, the vapor of the organic vapor deposition material 121 held by the vapor deposition source 120 and the vapor deposition source 141 held by the vapor deposition source 140 with the shutter 180 in the open state rises in the vacuum chamber 110 and passes through the opening of the substrate holder 190. A first antifogging organic film made of a mixed film of the organic vapor deposition material 121 and the organic vapor deposition material 141 is deposited on the surface of each glass lens 10 placed on the substrate holder 190.

  When the mixed film (first antifogging organic film) of the organic vapor deposition material 121 and the organic vapor deposition material 141 is formed, the opening 161 of the deposition preventing container 160 in which the vapor deposition source 130 is accommodated is provided with a shutter 180. Therefore, the vapor of the organic vapor deposition material 131 stays in the deposition chamber 160 and is not released into the vacuum chamber 110, thereby preventing the vapor deposition source 120 and the vapor deposition source 140 from being contaminated. Can do. Further, the vapors of the organic vapor deposition materials 121 and 141 released from the vapor deposition sources 120 and 140 do not contaminate the vapor deposition source 130.

Then, the motor 182 operates again, and the shutter 180 rotates with the rotation of the rotating shaft 181. The shutter 180 is rotated to the left by 120 °, which is a unit of two rotation angles, and stops at the position d (see FIG. 4D).
Thereby, the vapor deposition source 130 holding the organic vapor deposition material 131 and the vapor deposition source 140 holding the organic vapor deposition material 141 are opened, and the vapor deposition source 120 holding the organic vapor deposition material 121 is shielded.

  Then, the vapors of the second organic vapor deposition material 131 held in the second vapor deposition source 130 and the third organic vapor deposition material 141 held in the third vapor deposition source 140 in the vacuum chamber 110 are preliminarily heated. To be released. The emitted vapors of the second organic vapor deposition material 131 and the third organic vapor deposition material 141 rise in the vacuum chamber 110 and pass through the opening of the substrate holder 190 and onto the glass lens 10 placed on the substrate holder 190. A second antifogging organic film made of the mixed film of the second organic vapor deposition material 131 and the organic vapor deposition material 141 is deposited on the formed mixed film of the organic vapor deposition material 121 and the organic vapor deposition material 141. Is done.

  When the mixed film (second antifogging organic film) of the organic vapor deposition material 131 and the organic vapor deposition material 141 is formed, the opening 151 of the deposition preventing container 150 in which the vapor deposition source 120 is accommodated is provided with the shutter 180. Therefore, the vapor of the organic vapor deposition material 121 stays in the deposition vessel 150 and is not released into the vacuum chamber 110, thereby preventing the vapor deposition source 130 and the vapor deposition source 140 from being contaminated. Can do. Further, the vapor of the organic vapor deposition materials 131 and 141 released from the vapor deposition sources 130 and 140 does not contaminate the vapor deposition source 120.

Then, after vapor deposition of the second antifogging organic film is completed, power supply to the vapor deposition sources 120, 130, and 140 is stopped, and the inside of the vacuum chamber 110 is opened to the atmosphere and returned to atmospheric pressure.
Then, the substrate holder 190 on which the glass lens 10 is placed is taken out from the vacuum chamber 110, and the first antifogging organic film and the second antifogging organic film are formed on one lens surface. The obtained glass lens 10 is obtained. If necessary, an antifogging organic film is formed on the other lens surface of the glass lens 10 by the same operation method.

In addition, when the 1st anti-fogging organic film which consists of a mixed film of the organic vapor deposition material 121 and the organic vapor deposition material 141 is formed into a film, the organic vapor deposition material 121 and the organic vapor deposition material 141 which are hold | maintained at each vapor deposition source 120,140 are formed. By changing the ratio of the holding amount, the material composition of the first antifogging organic film formed by vapor deposition can be adjusted. The same applies to the second antifogging organic film.
Moreover, the film thickness of each antifogging organic film | membrane formed into a film can obtain a desired film thickness by controlling the open time of the shutter 180, ie, vapor deposition time.

  According to this vapor deposition example 1, the shutter 180 for opening and shielding the vapor | steam of the organic vapor deposition material 121,131,141 hold | maintained at three vapor deposition sources 120,130,140 is three vapor deposition sources 120,130,140. By having an open region in which one or two of 130 and 140 are simultaneously opened, two different types of organic vapor deposition materials can be deposited simultaneously. Thereby, the mixed film of the organic vapor deposition material that causes a chemical reaction by mixing two kinds of compositions in advance can be formed with high purity.

  Moreover, according to this vapor deposition example 1, the boiling points of three different types of organic vapor deposition materials 121, 131, 141 held in the three vapor deposition sources 120, 130, 140 of the vacuum vapor deposition apparatus 100 are close to each other. Therefore, a desired organic film (antifogging organic film) can be continuously formed. Therefore, it is possible to continuously form a multilayer organic film on the glass lens 10 while maintaining the vacuum state in the vacuum chamber 110, and the working efficiency of the vapor deposition process is improved.

  Further, when forming a mixed film of organic vapor deposition materials, even if two different types of organic vapor deposition materials adhere to each other's vapor deposition sources, they are heated to the temperature at which each organic vapor deposition material evaporates. Because it is not deposited. This means that even when the vapor deposition operation is completed and a new batch of vapor deposition is performed next, impurities do not remain in the vapor deposition source, and a new vapor deposition material can be deposited with high purity.

(Vapor deposition example 2)
In the deposition example 2, a plastic lens is used as the substrate 10, a mixed film made of a water-repellent organic material and an oil-repellent organic material is formed on the plastic lens, and a hydrophilic film made of a hydrophilic organic material is formed on the mixed film. It is an example of vapor deposition in the case of forming an organic film. In addition, the plastic lens 10 used that the inorganic antireflection film was formed in advance on the surface of the plastic lens substrate. Hereinafter, in the deposition example 2, the plastic lens is represented as a plastic lens 10 instead of the substrate 10.

The mixed film made of a water-repellent organic material and an oil-repellent organic material formed on the plastic lens 10 is an antifouling functional film, and when the lens is used, the lens surface is soiled by dirt, sweat, cosmetics, etc. It has the function of imparting antifouling performance to make it difficult to adhere and to easily wipe off dirt.
Further, the hydrophilic organic film formed on the mixed film is formed as a pretreatment of the antifogging treatment that imparts the antifogging function, and after these deposited films including the mixed film are formed, for example, an immersion method A surface active agent is applied using, and an antifogging functional film is formed.

  As the water repellent organic material, a fluorine-containing silane compound represented by the following general formula (1) was prepared as the first organic vapor deposition material 121. Specific examples thereof include “KP-801M” (trade name, manufactured by Shin-Etsu Chemical Co., Ltd.).

但し、式中、Ｒｆ¹は、パーフルオロアルキル基を表す。Ｚは、フッ素またはトリフルオロメチル基を表す。ａ、ｂ、ｃ、ｄ、ｅは、それぞれ独立して、０または１以上の整数を表し、ａ＋ｂ＋ｃ＋ｄ＋ｅは、少なくとも１以上であり、ａ、ｂ、ｃ、ｄ、ｅで括られた各繰り返し単位の存在順序は、式中において限定されない。Ｙは、水素または炭素数１〜４のアルキル基を表す。Ｘ¹は、水素、臭素またはヨウ素を表す。Ｒ¹は、水酸基または加水分解可能な置換基を表す。Ｒ²は、水素または１価の炭化水素基を表す。ｈは、０、１または２の何れかを表す。ｍは１、２または３の何れかを表す。ｎは、１以上の整数を表す。

However, in the formula, Rf ¹ represents a perfluoroalkyl group. Z represents a fluorine or trifluoromethyl group. a, b, c, d and e each independently represent 0 or an integer of 1 or more, a + b + c + d + e is at least 1 or more, and each repeating unit surrounded by a, b, c, d and e The order of presence of is not limited in the formula. Y represents hydrogen or an alkyl group having 1 to 4 carbon atoms. X ¹ represents hydrogen, bromine or iodine. R ¹ represents a hydroxyl group or a hydrolyzable substituent. R ² represents hydrogen or a monovalent hydrocarbon group. h represents 0, 1 or 2. m represents either 1, 2 or 3. n represents an integer of 1 or more.

  For the oil-repellent organic material, a fluorine-containing silane compound (perfluoropolyalkylene ether-modified silane) represented by the following general formula (2) was prepared as the second organic vapor deposition material 131. Specific examples thereof include “KY-130” (trade name, manufactured by Shin-Etsu Chemical Co., Ltd.).

但し、式中、Ｒｆ²は、式：「−（Ｃ_kＦ_2k）Ｏ−」（式中、ｋは１〜６の整数である）で表される単位を含み、分岐を有しない直鎖状のパーフルオロポリアルキレンエーテル構造を有する２価の基を表す。Ｒ³は炭素原子数１〜８の一価炭化水素基であり、Ｘ²は加水分解性基またはハロゲン原子を表す。ｓは０、１または２の何れかを表す。ｔは１〜５の整数を表す。ｈおよびｉは２または３を表す。

However, in the formula, Rf ² includes a unit represented by the formula: “— (C _k F _2k ) O—” (wherein k is an integer of 1 to 6), and is a straight chain having no branch. Represents a divalent group having a perfluoropolyalkylene ether structure. R ³ is a monovalent hydrocarbon group having 1 to 8 carbon atoms, and X ² represents a hydrolyzable group or a halogen atom. s represents either 0, 1 or 2. t represents an integer of 1 to 5. h and i represent 2 or 3.

  The mixed film formed by using the fluorine-containing silane compound represented by the general formula (1) or the general formula (2) has high antifouling performance, scratch resistance, wiping properties, chemical resistance, etc. Antifouling performance with improved durability can be obtained. The boiling points of the water-repellent organic material (first organic vapor deposition material 121) and the oil-repellent organic material (second organic vapor deposition material 131) are both about 550 ° C. (530 ° C. to 560 ° C.).

  As the third organic vapor deposition material 141, the hydrophilic organic material includes 3-mercaptopropyltriethoxysilane, 3-mercaptopropyltrimethoxysilane, 2-mercaptopropyltrimethoxysilane, 2-mercaptopropyltriethoxysilane, 2-mercapto. A silane coupling agent having a thiol group, such as ethyltrimethoxysilane or 2-mercaptoethyltriethoxysilane, alone or a mixture of two or more of these may be used. The boiling point of these hydrophilic organic materials (third organic vapor deposition material 141) is about 80 ° C.

  In the vacuum deposition method on the plastic lens 10, first, the prepared plastic lens 10 was placed on a large number of openings of the substrate holder 190 previously removed from the holder rotating shaft 191 of the vacuum deposition apparatus 100. Then, the substrate holder 190 on which the plastic lens 10 was placed was held in the vacuum chamber 110 and attached to the holder rotating shaft 191.

  On the other hand, the first organic vapor deposition material 121 is charged and held in the first vapor deposition source 120 (boat type container). Similarly, the second organic vapor deposition material 131 is held in the second vapor deposition source 130, and the third organic vapor deposition material 141 is held in the third vapor deposition source 140.

After the organic vapor deposition material 121, the organic vapor deposition material 131, and the organic vapor deposition material 141 are held in the respective vapor deposition sources (boat-type containers), the motor 182 operates to rotate the shutter 180 along with the rotation of the rotating shaft 181. The shutter 180 rotates at a predetermined position of the shutter 180 (center line of the outer shape δ portion, see FIG. 3) to the position b, and stops at the position b (see FIG. 4B).
Thereby, the vapor deposition source 120 holding the organic vapor deposition material 121 and the vapor deposition source 130 holding the organic vapor deposition material 131 are opened, and the vapor deposition source 140 holding the organic vapor deposition material 141 is blocked.

Then, a vacuum pump combining a dry pump and a turbo molecular pump is operated, and the inside of the vacuum chamber 110 is exhausted to an ultimate pressure of about 1 × 10 ⁻² Pa through an exhaust port 111 formed on the side wall of the vacuum chamber 110. The

  Then, the holder rotating motor 192 is driven to rotate the substrate holder 190 on which a large number of plastic lenses 10 are placed, and an electric current is supplied to the vapor deposition sources 120 and 130 so that the boat-type container generates resistance heat. The organic vapor deposition materials 121 and 131 generated and held in the vapor deposition sources 120 and 130 are heated. The temperature at which the organic vapor deposition materials 121 and 131 are heated is about 600 ° C.

  As a result, the vapors of the vapor deposition source 120 holding the organic vapor deposition material 121 and the vapor deposition source 130 holding the organic vapor deposition material 131 with the shutter 180 in the open state rise in the vacuum chamber 110 and pass through the opening of the substrate holder 190. An antifouling functional film made of a mixed film of the organic vapor deposition material 121 and the organic vapor deposition material 131 is deposited on the surface of each plastic lens 10 placed on the substrate holder 190.

  When the mixed film of the organic vapor deposition material 121 and the organic vapor deposition material 131 is formed, since the opening 171 of the deposition preventing container 170 in which the vapor deposition source 140 is accommodated is shielded by the shutter 180, the organic vapor deposition material. 141 is not contaminated.

  Then, power supply to the vapor deposition sources 120 and 130 used to form the antifouling functional film is stopped, and a current is passed through the third vapor deposition source 140 holding the third organic vapor deposition material 141. The boat-type container generates resistance heat, and the organic vapor deposition material 141 is heated. The temperature at which the organic vapor deposition material 141 is heated is about 100 ° C.

Then, the motor 182 operates again, and the shutter 180 rotates with the rotation of the rotating shaft 181. The shutter 180 is rotated to the left by 60 °, which is a rotation angle unit, at a predetermined position of the shutter 180, and stops at the position a (see FIG. 4A).
Thereby, the vapor deposition source 120 holding the organic vapor deposition material 121 and the vapor deposition source 130 holding the organic vapor deposition material 131 are shielded, and the vapor deposition source 140 holding the organic vapor deposition material 141 is opened.

  Then, the vapor of the third organic vapor deposition material 141 held by the third vapor deposition source 140 and heated is released into the vacuum chamber 110. The vapor of the third organic vapor deposition material 141 released from the third vapor deposition source 140 rises in the vacuum chamber 110 and is placed on the substrate holder 190 through the opening of the substrate holder 190. A hydrophilic organic film made of the third organic vapor deposition material 141 is formed on the antifouling functional film made of a mixed film of the organic vapor deposition material 121 and the organic vapor deposition material 131 formed on the surface.

  When the organic vapor deposition material 141 is formed, the opening 151 of the deposition preventing container 150 in which the deposition source 120 is accommodated and the opening 161 of the deposition preventing container 160 in which the deposition source 130 is accommodated are shielded by the shutter 180. Therefore, the vapor of the organic vapor deposition material 141 released from the vapor deposition source 140 does not contaminate the vapor deposition sources 120 and 130. Moreover, the boiling point of the organic vapor deposition material 141 is much lower than that of the first organic vapor deposition material 121 and the second organic vapor deposition material 131 previously formed, and the heating temperature is low. Even when 131 is deposited around the vapor deposition source 140 including the deposition preventing container 170, the organic vapor deposition materials 121 and 131 are not contaminated.

And after vapor deposition of the 3rd organic vapor deposition material 141 is complete | finished, while stopping the electric power feeding of the vapor deposition source 140, the inside of the vacuum chamber 110 is open | released to air | atmosphere, and it returns to atmospheric pressure.
Then, the substrate holder 190 on which the plastic lens 10 is placed is taken out from the vacuum chamber 110, and the plastic lens 10 in which the antifouling functional film and the hydrophilic organic film are formed on one lens surface is obtained. can get.

Thereafter, an antifouling functional film and a hydrophilic organic film are formed on the other lens surface of the plastic lens 10 by the same vapor deposition method as described above to form an antifogging organic film.
According to the deposition example 2, the same effect as the deposition example 1 can be obtained.

  The vacuum vapor deposition apparatus of the present invention is not limited to the above-described embodiment, and the same effects as those of the embodiment can be obtained even in the form described below.

  (1) Resistance heating evaporation using a boat-type container that generates resistance heat when an electric current is applied as the three evaporation sources 120, 130, and 140 disposed in the vacuum chamber 110 of the vacuum evaporation apparatus 100. As described in the case of the source, any resistance heating method may be used, for example, indirect resistance heating method in which the outer peripheral side surface of the crucible is heated with a heater instead of a boat-type container, or lamp heating using a halogen lamp or the like. It may be a case where a method is used. When the organic vapor deposition material is vacuum-deposited, it is preferable to use a resistance heating vapor deposition source as the vapor deposition source, but an electron beam vapor deposition method in which the organic vapor deposition material is vaporized by the energy of the electron beam can also be used.

  (2) Between the deposition source 120, 130, 140 disposed in the vacuum chamber 110 and the substrate holder 190 on which the substrate 10 (glass lens or plastic lens) to be deposited is placed, A correction plate for correcting the distribution of the deposited film thickness may be disposed substantially in parallel. In addition, a film thickness detection device for detecting the film thickness of the organic thin film to be formed can be provided.

  (3) Although the number of vapor deposition sources arranged in the vacuum chamber 110 of the vacuum vapor deposition apparatus 100 has been described in the case where three vapor deposition sources are arranged, when the area of the bottom surface of the vacuum chamber 110 is large, Based on the technical idea of the present embodiment, three or more plural pieces are respectively arranged on two or two or more circumferences having different distances from the rotation center O of the rotation shaft 181, and the shutter 180. By considering the outer shape, one or two of the plurality of vapor deposition sources can be simultaneously opened.

1 is a side sectional view showing an outline of a vacuum vapor deposition apparatus of the present invention. FIG. 2 is an arrow view of a cross section taken along line AA of the vacuum vapor deposition apparatus shown in FIG. 1. Sectional drawing of the vacuum evaporation system which looked at the bottom face direction of the vacuum chamber. Sectional drawing of the vacuum evaporation system which looked at the bottom face direction of the vacuum chamber which shows the aspect in the stop position for every rotation angle unit of a shutter.

Explanation of symbols

  DESCRIPTION OF SYMBOLS 10 ... Glass lens, plastic lens as a substrate, 100 ... Vacuum vapor deposition apparatus, 110 ... Vacuum chamber, 111 ... Exhaust port, 120, 130, 140 ... Deposition source, 121, 131, 141 ... Organic vapor deposition material, 150, 160, 170 ... Anti-adhesion container, 151,161,171 ... An opening of the anti-adhesion container, 180 ... Shutter, 181 ... Rotation shaft, 182 ... Motor, 190 ... Substrate holder, 191 ... Holder rotation shaft, 192 ... For holder rotation Motor, DA, DB, DC: Area covering the opening, O: Center of rotation of the rotation axis, θ: Arrangement angle, β: Unit of rotation angle.

Claims (4)

A vacuum deposition apparatus for forming a thin film made of an organic compound on a substrate,
A vacuum chamber, a plurality of vapor deposition sources for individually holding different types of organic compounds in the vacuum chamber, and a plurality of vapor deposition sources between the plurality of vapor deposition sources and the substrate. A shutter for opening and shielding the vapor of the organic compound formed,
The vacuum deposition apparatus, wherein the shutter has an open region that simultaneously opens two of the plurality of deposition sources, and rotates about the center of the vacuum chamber as a rotation axis. In the vacuum evaporation system according to claim 1,
The plurality of vapor deposition sources are disposed at substantially equal angles with respect to the rotation center of the shutter,
The shutter rotates about the rotation axis, and the open region simultaneously opens one or two of the plurality of vapor deposition sources, and the other vapor deposition sources excluding the opened vapor deposition sources. A vacuum vapor deposition apparatus characterized by shielding. In the vacuum evaporation system according to claim 2,
The vacuum deposition apparatus according to claim 1, wherein the shutter is rotatable in units of ½ of the arrangement angle where the plurality of deposition sources are arranged. In the vacuum evaporation system as described in any one of Claims 1-3,
2. The vacuum deposition apparatus according to claim 1, wherein at least two of the plurality of deposition sources are held by a deposition source that is simultaneously opened by the shutter, and the organic compounds of different types are close to each other in boiling point.

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