JP2005325400A - Vacuum deposition system and thin film deposition method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To correctly monitor the film thickness of a vapor-deposited metal apt to resublimate at the time of vapor-depositing the metal. <P>SOLUTION: A metal fixing material is beforehand vapor-deposited on the surface 13a of a quartz resonator 13 provided at a film thickness monitor 12, thereafter, alkali metal is vapor-deposited on an organic compound layer in a stacked body S1 as a example of the object to be vapor-deposited and on the surface 13a of the quartz resonator 13 with the metal fixing material vapor-deposited. The alkali metal vapor-deposited on the quartz resonator 13 is reacted with the metal fixing material, and hardly resublimates. The film thickness of the alkali metal measured with the film thickness monitor 12 is made equal to the film thickness of the alkali metal vapor-deposited on the organic compound layer in the stacked body S1. By monitoring the film thickness of the alkali metal with the film thickness monitor 12, the film thickness of the alkali metal vapor-deposited on the organic compound layer can be correctly detected. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a technical field of a vacuum deposition apparatus and a thin film forming method suitable for doping a metal into an organic compound layer included in an organic EL element, for example.

  In an organic EL (Electroluminescence) element, a light emitting layer, which is an organic thin film made of at least one organic compound, is formed on one electrode film formed together with wirings and elements on a substrate, and another electrode is further formed thereon. A film is formed. In order to efficiently inject charges from each electrode to the light emitting layer, a charge injection layer may be formed between each electrode film and the light emitting layer.

  For example, according to Patent Document 1, in an organic EL element having at least one light emitting layer composed of an organic compound between an opposing anode and cathode, a metal doping layer is provided between the light emitting layer and the cathode. ing. The metal doped in the metal doping layer functions as a donor dopant.

  Patent Document 1 describes that the above-described element structure reduces the electron injection barrier from the cathode to the organic compound layer, leading to improvement in element characteristics. Since the metal doping layer does not increase the driving voltage of the organic EL element even if the layer thickness is increased, Patent Document 1 discloses an optical layer thickness (layer) between the cathode and the light emitting layer that acts as a reflecting mirror. It also describes a technique for expressing a light interference effect by changing the thickness of the optical path length (layer thickness × refractive index), and control of the emission spectrum using this technique. The metal used for the metal doping layer is composed of one or more of transition metals including alkali metals, alkaline earth metals, and rare earth metals having a work function of 4.2 eV or less. Vapor deposited on the layer.

  The vacuum vapor deposition apparatus used for forming the doping layer includes a film thickness monitor using a crystal resonator in a vapor deposition chamber, and vapor deposition material evaporated by being heated by a vapor deposition source adheres to the crystal resonator. . The film thickness monitor can measure the film thickness of the metal deposited on the crystal resonator based on the weight change of the metal attached to the crystal resonator. The vacuum deposition apparatus detects the thickness of the metal deposited on the crystal resonator as the thickness of the metal deposited on the organic compound layer.

JP 2001-102175 A

  However, many metals used for the metal doping layer have a low melting point and boiling point. For example, cesium (Cs), which is an alkali metal, has a melting point of 28.4 ° C. and a boiling point of 678.4 ° C. Even if Cs is vaporized in the vacuum vapor deposition apparatus and vapor-deposited on the crystal resonator, the cesium vapor deposited on the crystal resonator is readily vaporized under high vacuum in the vacuum vapor deposition apparatus. Therefore, the film thickness of Cs deposited on the crystal unit does not match the film thickness of Cs deposited on the organic compound layer, and the crystal unit type film thickness monitor stably measures the film thickness. It is difficult. As described above, the crystal oscillator type film thickness monitor has a problem that it is difficult to accurately detect the film thickness of Cs deposited on the organic compound layer.

  In order to measure the thickness of the alkali metal, it may be possible to use a deposition rate monitor using atomic absorption, but adding an atomic absorption spectrometer in addition to the vacuum deposition device This causes disadvantages such as an increase in the size of the apparatus and an increase in cost.

  Therefore, the present invention has been made in view of the above problems. For example, in an organic EL element, when an organic compound layer such as an electron injection layer is doped with an alkali metal, the organic compound layer is deposited on the organic compound layer. It is an object of the present invention to provide a vacuum vapor deposition apparatus and a vacuum vapor deposition method that make it possible to accurately measure the thickness of an alkali metal, and that hardly increase the size and cost of the apparatus.

In order to solve the above problems, a vacuum vapor deposition apparatus according to the present invention has a metal vapor deposition means for vapor-depositing a metal having a low boiling point temperature on a vapor deposition target, and before or after vapor deposition of the metal on the vapor deposition target. When the metal is deposited on the deposition target, the metal fixing material for fixing the metal is fixed to the metal fixing material on the deposition target surface. Measuring means for measuring the thickness of the metal deposited on the deposition target based on the weight change of the metal.

  According to the vacuum evaporation apparatus according to the present invention, for example, a metal having a low boiling point temperature such as an alkali metal is applied to an evaporation target such as an organic compound layer such as an organic EL element by a metal evaporation means provided in a vacuum chamber. Is deposited. Here, the “deposition target” according to the present invention means an object on which a vapor deposition film is formed by the deposition of the metal vaporized by the metal vapor deposition means. On the other hand, it means a substrate disposed oppositely or a layer formed on the substrate. In addition, the “metal having a low boiling point temperature” according to the present invention does not only mean that it has a boiling point temperature or a sublimation point temperature at room temperature or below room temperature under high vacuum in a vacuum vapor deposition apparatus, but is vapor deposited by metal vapor deposition means. Means a metal having a boiling point temperature or sublimation point temperature below the temperature of the atmosphere in which That is, the “low boiling point temperature” according to the present invention is relatively low with respect to the film formation temperature or the atmospheric temperature during film formation on the deposition target related to the metal vapor deposition means, It means the temperature at which vaporization occurs. Examples of such “low-boiling temperature metals” include alkali metals. In addition to Cs, examples include lithium (Li), sodium (Na), potassium (K), and rubidium (Rb). it can. Moreover, as a metal vapor deposition means, the vapor deposition means by the resistance heating vapor deposition method, the electromagnetic heating vapor deposition method, etc. is employ | adopted, for example.

  In parallel with the vapor deposition by such a metal vapor deposition means, for example, a metal film deposited on a deposition target by a measurement means such as a crystal oscillator type film thickness monitor disposed in a vacuum chamber where vapor deposition is performed. Thickness is measured. This measurement is performed as follows.

  That is, when low-boiling point metal is vapor-deposited by the metal vapor-depositing means, a low-boiling-point metal is also vapor-deposited on the surface to be vapor-deposited in the measuring means such as the surface of a crystal resonator. Here, in particular, a metal fixing material for fixing the low boiling point metal is deposited on the deposition surface of the measuring means before the low boiling point metal is deposited in advance. Here, as the “metal fixing material” according to the present invention, for example, it is easy to deposit under a predetermined pressure in the chamber, and the complex is formed by reacting with a metal having a low boiling point such as an alkali metal. An organic compound such as an organic chelate compound that is easily formed can be used. Therefore, at the time of vapor deposition, the low boiling point metal reacts with the metal fixing material on the vapor deposition surface of the measuring means, and the reacted metal is the vapor deposition surface even if it is a low boiling point metal. Almost no resublimation or vaporization. In other words, the film thickness of the low boiling point metal fixed on the surface to be deposited in this way is almost identical to the film thickness of the low boiling point metal deposited on the deposition target in almost or practical sense. become. Moreover, even if a metal having a low boiling point temperature is not sublimated or vaporized on the deposition surface of the measuring means, the weight change of the low boiling point metal film formed on the deposition surface by the measuring means is stable. Will be measured.

  As a result, even when the metal has a low boiling point, it is possible to control the film thickness with high accuracy by accurately measuring the film thickness of the metal deposited on the deposition target. Furthermore, since it is not necessary to separately provide a film thickness measuring device such as an atomic absorption spectrum meter device, it is possible to suppress an increase in the size of the device and to reduce the cost for introducing new equipment. It becomes possible.

  In addition, in the vacuum deposition apparatus according to the present invention, it is not limited to the target to be deposited before vapor deposition of the metal having a low boiling point, and simultaneously or alternately when depositing the alkali metal on the organic compound layer, A metal fixing material may be vapor-deposited on the deposition surface of the measuring means, and both the low boiling point metal and the metal fixing material may be deposited on the deposition surface of the measuring means. The low boiling point metal is fixed to this surface in a state of reacting with the metal fixing material by depositing the low boiling point metal and the metal fixing material simultaneously or almost simultaneously on the deposition surface of the measuring means. .

  In one aspect of the vacuum vapor deposition apparatus according to the present invention, when the metal fixing material is vapor-deposited on the surface to be vapor-deposited, the vapor deposition inhibiting means inhibits the metal fixing material from being vapor-deposited on the vapor deposition target. May be provided.

  According to this aspect, the vapor deposition inhibiting unit can suppress the metal fixing material from being deposited on the deposition target, and the metal fixing material is deposited only on the deposition target surface. Therefore, when the metal fixing material is vapor-deposited on the deposition target surface, it is possible to reduce the adhesion of the metal fixing material to the organic compound layer which is an example of the deposition target. For example, the organic compound layer is provided. It is possible to suppress degradation of element characteristics of the organic EL element that is configured. Thus, when it is not preferable that the metal fixing material is deposited on the deposition target, the vacuum deposition apparatus according to this aspect is a suitable apparatus for performing deposition. As the vapor deposition inhibiting means, for example, a partition plate that blocks the flow of the gas can be used so that the gas of the metal fixing material does not flow around the deposition target.

  In another aspect of the vacuum evaporation apparatus according to the present invention, a temperature adjusting unit that adjusts a temperature of the measuring unit may be provided when measuring the film thickness of the metal fixed to the metal fixing material. .

  According to this aspect, the temperature adjusting unit can reduce the influence of the ambient temperature on the measuring unit, and the measuring unit can accurately measure the film thickness of the low boiling point metal deposited on the deposition target. . For example, a measuring means such as a crystal oscillator type film thickness monitor can accurately measure the weight change of the metal deposited on the crystal oscillator even when the ambient temperature of the crystal oscillator changes. The film thickness of the metal obtained based on the change corresponds to the film thickness of the metal deposited on the deposition target. As the temperature adjusting means, for example, a water-cooling type temperature adjusting device may be mentioned.

  In another aspect of the vacuum vapor deposition apparatus according to the present invention, a metal fixing material vapor deposition means for depositing the metal fixing material on the deposition surface, an operation of the metal vapor deposition means, and an operation of the metal fixing material vapor deposition means. And the metal vapor deposition means and the metal fixing material vapor deposition means provided in the same chamber are controlled by the control means to deposit the metal on the deposition target. And vapor deposition of the metal fixing material on the surface to be vapor-deposited.

  According to this aspect, the metal fixing material is applied to the deposition surface at a stage where the laminate including the deposition target such as the organic compound layer is not put into the chamber under the control of the control unit which is an example of the control unit. Evaporate. Subsequently, only the metal can be deposited on the organic compound layer by putting the laminate into the chamber and evaporating the metal from a metal deposition means such as a deposition source. Even when the metal vapor deposition means and the metal fixing material vapor deposition means are not arranged in the partitioned spaces in the same chamber, the vapor deposition of the metal to the vapor deposition target and the metal fixation to the vapor deposition surface are controlled under the control of the control unit. The metal fixing material does not adhere to the organic compound layer by performing the vapor deposition of the material one after the other. Therefore, it is not necessary to provide a new device for switching the deposition of the metal fixing material and the low boiling point metal, and the thickness of the metal deposited on the organic compound layer can be accurately determined without complicating the device configuration. The thickness of the metal can be controlled while detecting.

  In this aspect, when the metal deposition means deposits the metal on the deposition target, the metal fixing material deposition means may deposit the metal fixing material on the deposition surface.

  According to this aspect, the low boiling point metal and the metal fixing material that reacts with the metal can be simultaneously deposited on the deposition surface. For example, an alkali metal, which is an example of a metal having a low boiling point, and an organic compound compound, which is an example of a metal fixing material, can be deposited simultaneously.

  Once the organic metal compound is deposited and then the alkali metal is deposited, the alkali metal deposited on the alkali metal thin film is easily sublimated without reacting with the organic compound. The film thickness of the alkali metal actually deposited on the surface to be deposited becomes thinner than the film thickness of the alkali metal deposited on the deposition target, and the thickness of the alkali metal deposited on the deposition target is accurately measured by the measuring means. It may be difficult to detect.

  Therefore, by simultaneously depositing the alkali metal and the organic chelate compound on the deposition surface, it is possible to react and fix all of the deposited alkali metal with the organic chelate compound on the deposition surface. Since almost no alkali metal is resublimated from the deposition surface, the thickness of the alkali metal deposited on the deposition target is equal to the thickness of the alkali metal deposited on the deposition surface. Therefore, by measuring the thickness of the alkali metal deposited on the deposition surface, that is, the change in weight, it is possible to accurately measure the thickness of the alkali metal deposited on the deposition target.

  In order to solve the above problems, a thin film forming method according to the present invention deposits a metal having a low boiling point temperature on a deposition target, and before or when depositing the metal on the deposition target. A metal fixing material deposition step for depositing a metal fixing material for immobilizing the metal on a deposition surface different from the deposition target; and when the metal is deposited on the deposition target, the deposition target A measuring step of measuring a film thickness of the metal deposited on the deposition target based on a change in weight of the metal fixed to the metal fixing material on the surface.

  According to the thin film forming method of the present invention, first, a low boiling point metal is vapor-deposited on a deposition target by a metal vapor deposition means. A metal fixing material for fixing a metal having a low boiling point temperature is deposited on the deposition surface of the measuring means. Therefore, the low boiling point metal is deposited on the deposition target and deposited on the deposition surface on which the metal fixing material is deposited. The low boiling point metal that has reacted with the metal fixing material on the deposition surface is hardly sublimated or vaporized from the deposition surface even if it is a low boiling point metal. In other words, the film thickness of the low boiling point metal fixed on the surface to be deposited in this way is almost identical to the film thickness of the low boiling point metal deposited on the deposition target in almost or practical sense. become. In addition, even if a metal having a low boiling point temperature is not resublimated or vaporized on the deposition surface of the measuring means, the weight change of the low boiling point metal film formed on the deposition surface by the measuring means is stable. Will be measured.

  In addition, in the vacuum deposition apparatus according to the present invention, it is not limited to the target to be deposited before vapor deposition of the metal having a low boiling point, and simultaneously or alternately when depositing the alkali metal on the organic compound layer, A metal fixing material may be vapor-deposited on the deposition surface of the measuring means, and both the low boiling point metal and the metal fixing material may be deposited on the deposition surface of the measuring means. The low boiling point metal is fixed to this surface in a state of reacting with the metal fixing material by depositing the low boiling point metal and the metal fixing material simultaneously or almost simultaneously on the deposition surface of the measuring means. .

  Such an operation and other advantages of the present invention will become apparent from the embodiments described below.

  Hereinafter, embodiments of the present invention will be described with reference to the drawings. In the following embodiments, the vacuum vapor deposition apparatus of the present invention is applied to an organic EL element manufacturing apparatus.

(First embodiment)
FIG. 1 is a diagram schematically showing a vacuum vapor deposition apparatus according to the first embodiment.

  In FIG. 1, a vacuum vapor deposition apparatus 10 according to this embodiment includes a chamber 11, a film thickness monitor 12, vapor deposition units 14 and 15, a support unit 16, a partition plate 17, and a control unit 18.

  The chamber 11 is a vacuum chamber for depositing an alkali metal, which is an example of the “metal having a low boiling point temperature” according to the present invention, on the stacked body S1. In the chamber 11, a film thickness monitor 12, a support portion 16 that supports the film thickness monitor 12, vapor deposition units 14 and 15, and a partition plate 17 are disposed.

  The stacked body S1 constitutes a part of an organic EL element formed by stacking a plurality of organic compound layers. The organic compound layer, which is an example of the “deposition target” according to the present invention, is one of the organic compound layers provided in the stacked body S1, and improves at least one of the electron injection efficiency and the electron transport property from the cathode to the light emitting layer. This is an organic compound layer provided for the purpose. The stacked body S <b> 1 is put into the chamber 11 so that the surface of the organic compound layer faces the vapor deposition unit 14. In the present embodiment, although the detailed configuration of the stacked body S1 is not illustrated, the stacked body S1 may be an organic EL element in which a plurality of organic compound layers are formed on a substrate, and a plurality of organic EL elements are formed. For this purpose, a plurality of laminated bodies may be formed on the substrate. According to the vacuum deposition apparatus according to the present embodiment, when forming a plurality of organic EL elements, it is possible to simultaneously deposit an alkali metal on an organic compound layer such as an electron injection layer provided in each organic EL element, An element having excellent characteristics with respect to at least one of electron injection efficiency and electron transportability can be efficiently formed.

  The “evaporation target” according to the present invention is not limited to the organic compound layer provided in order to increase at least one of the electron injection efficiency and the electron transport property. Anything can be used. The “deposition target” according to the present invention may be, for example, a vacuum vessel provided in a cathode ray tube, a plasma display, a fluorescent display tube, a thermos bottle, or the like. The performance of such a vacuum vessel depends on the pressure in the vessel and the residual gas. Therefore, by depositing a gas adsorbing material called a getter material or a gettering material in the container, impurities that are one of the causes of lowering the degree of vacuum in the container can be adsorbed. In some cases, an alkali metal is used as the getter material. According to the vacuum deposition apparatus 10 according to the present embodiment, such a getter material can be easily deposited on the vacuum vessel, and the film thickness of the getter material can be accurately measured. It is also possible to control well.

  The alkali metal is heated by the vapor deposition unit 14, and the vaporized alkali metal is vapor-deposited on the organic compound layer of the laminate S1. Alkali metals deposited to increase at least one of the electron transport property and the electron injection efficiency of the organic EL element are, for example, cesium (Cs), lithium (Li), sodium (Na), potassium (K), rubidium (Rb). ) Etc. These alkali metals are metals that easily sublimate even if they are once deposited when vacuum deposition is performed. For example, Cs has a melting point of 28.4 ° C. and a boiling point of 678.4 ° C.

  The vapor deposition unit 14, which is an example of the “metal vapor deposition means” according to the present invention, is disposed so as to face the stacked body S <b> 1 put into the chamber 11. Although a plurality of vapor deposition units 14 are provided in the vacuum vapor deposition apparatus 10, one vapor deposition unit 14 may be provided in the vacuum vapor deposition apparatus 10. The alkali metal gas evaporated from the vapor deposition unit 14 moves from the vapor deposition unit 14 toward the stacked body S1, and is deposited on the organic compound layer of the stacked body S1. In order to uniformly deposit the alkali metal on the organic compound layer, for example, by rotating the stacked body S1 with the deposition unit 14 being offset from the center of the stacked body S1, the entire organic compound layer of the stacked body S1 is rotated. It is also possible to form a film uniformly. You may adjust the distance of the laminated body S1 and the vapor deposition unit 14 so that an alkali metal may adhere to the laminated body S1 uniformly.

  The film thickness monitor 12 as an example of the “measurement means” according to the present invention is a crystal oscillator type film thickness monitor. The film thickness monitor 12 indicates the film thickness of the alkali metal deposited on the surface 13a based on the weight change of the alkali metal deposited on the surface 13a of the crystal resonator 13 which is an example of the “deposition surface” according to the present invention. measure. The vibration frequency of the crystal resonator 13 changes according to the change in the weight of the deposit attached to the surface 13a. Based on the change in frequency, the film thickness monitor 12 can measure the film thickness of the alkali metal deposited on the surface 13a.

  A metal fixing material for fixing the alkali metal is vapor-deposited on the surface 13a of the crystal unit 13 in advance before the alkali metal is vapor-deposited. The alkali metal reacts with the metal fixing material and is fixed to the surface 13 a of the crystal resonator 13. The alkali metal fixed to the metal fixing material is fixed to the surface 13a with almost no sublimation.

  The vapor deposition unit 14 vapor-deposits an alkali metal on the surface 13a on which the metal fixing material is vapor-deposited when vapor-depositing the alkali metal on the organic compound layer of the stacked body S1. Alkali metal that reacts with the metal fixing material on the surface 13a hardly resublimates, so the film thickness of the alkali metal deposited on the organic compound layer of the laminate S1 and the alkali metal deposited on the surface 13a of the crystal unit 13 It becomes equal to the film thickness. Therefore, it is possible to detect the thickness of the alkali metal measured by the thickness monitor 12 as the thickness of the alkali metal deposited on the organic compound layer of the stacked body S1.

  The vapor deposition unit 15, which is an example of the “metal fixing material vapor deposition unit” according to the present invention, vapor deposits the metal fixing material on the surface 13 a of the crystal resonator 13. The vapor deposition unit 15 is provided so as to face the film thickness monitor 12 including the crystal resonator 13. In this embodiment, the vapor deposition unit 15 is provided on the vertical line of the surface 13a of the crystal unit 13 provided in the crystal unit 13 more specifically. Therefore, the metal fixing material vaporized from the vapor deposition unit 15 rises toward the surface 13a of the crystal resonator 13 and is vapor deposited on the surface 13a as it is.

  The vapor deposition unit 15 vapor-deposits a metal fixing material before alkali metal is vapor-deposited on the surface 13 a of the crystal resonator 13. Before the alkali metal is vapor-deposited on the organic compound layer of the laminated body S1, the metal fixing material is vapor-deposited in advance on the crystal resonator 13, thereby reducing the resublimation of the alkali metal vapor-deposited on the surface 13a. The alkali metal is deposited on the surface 13a with a film thickness equal to that of the alkali metal deposited on the organic compound layer of the stacked body S1.

  In addition, when the vapor deposition unit 14 vapor-deposits an alkali metal on the organic compound layer of the laminated body S1, the vapor deposition unit 15 may vapor-deposit the metal fixing material on the crystal unit 13. By simultaneously depositing the alkali metal and the metal fixing material on the surface 13a of the crystal unit 13, the alkali metal sequentially deposits on the surface 13a while reacting with the metal fixing material. Compared with the case where a metal fixing material is vapor-deposited on the surface 13a in advance and only the alkali metal is vapor-deposited thereon, the alkali metal that does not react with the metal fixing material can be reduced. Accordingly, it is possible to suppress a decrease in film thickness due to resublimation of alkali metal once deposited on the surface 13a of the crystal resonator 13, and to stably measure the film thickness of alkali metal deposited on the organic compound layer. can do.

  The partition plate 17, which is an example of the “deposition inhibition unit” according to the present invention, is disposed between the vapor deposition unit 14 and the vapor deposition unit 15 and inhibits the gas flow of the metal fixing material toward the stacked body S <b> 1. . Therefore, the gas of the metal fixing material vaporized by the vapor deposition unit 15 is not vapor-deposited on the organic compound layer of the multilayer body S1, and the metal fixing material can be vapor-deposited on the surface 13a of the crystal resonator 13. The upper end of the partition plate 17 is set low with respect to the position of the film thickness monitor 12 so that the surface 13a of the crystal unit 13 faces the vapor deposition unit 14, and the flow of the alkali metal gas evaporated from the vapor deposition unit 14 Is not blocked by the partition plate 17. The partition plate 17 prevents the gas of the metal fixing material from flowing toward the stacked body S <b> 1 and prevents the alkali metal vaporized by the vapor deposition unit 14 from being deposited on the surface 13 a of the crystal resonator 13. Absent.

  The temperature adjustment device 20, which is an example of the “temperature adjustment means” according to the present invention, is provided on the support portion 16 that supports the film thickness monitor 12. The temperature adjustment device 20 is, for example, a water-cooled temperature adjustment device, and circulates cooling water using the film thickness monitor 12 to maintain the temperature of the crystal unit 13 constant. The crystal resonator 13 whose temperature is maintained constant is not affected by changes in the ambient temperature, and vibrates accurately at a frequency corresponding to the change in the weight of the alkali metal deposited on the surface 13a of the crystal resonator 13. To do. Therefore, even when the temperature in the vacuum deposition apparatus 10 changes, the film thickness monitor 21 can accurately measure the film thickness of the alkali metal deposited on the organic compound layer of the stacked body S1.

  The pump 19 exhausts the gas in the chamber 11 when performing vacuum vapor deposition, and sets the inside of the chamber 11 to a required degree of vacuum.

  The control unit 18 controls the operations of the vapor deposition units 14 and 15, the temperature adjustment device 20, and the film thickness monitor 12. The control unit 18 controls alkali metal deposition by the vapor deposition unit 14 and metal deposition by the vapor deposition unit 15. The controller 18 can switch the operation of the vapor deposition units 14 and 15. For example, the vapor deposition unit 14 can be stopped when the vapor deposition unit 15 is in operation, and the vapor deposition unit 15 can be stopped when the vapor deposition unit 14 is in operation. According to the control unit 18, the vapor deposition units 14 and 15 can be operated one after the other. After the metal fixing material is vapor deposited on the crystal resonator 13, the alkali metal is applied to the stacked body S <b> 1 and the crystal resonator 13. Vapor deposition can be performed. The control unit 18 can also operate the vapor deposition units 14 and 15 at the same time, and can perform vapor deposition of the alkali metal and the metal fixing material on the surface 13a of the crystal resonator 13 simultaneously. The control unit 18 can also control the pump 19 and control the transport device when transporting the stacked body S1 into the chamber 11.

  FIG. 2 is a diagram schematically showing the steps of the vacuum vapor deposition method using the vacuum vapor deposition apparatus 10 according to the first embodiment.

In FIG. 2A, the stacked body S <b> 1 is put into the chamber 11, and the gas in the chamber 11 is exhausted by the pump 19. In a state where the degree of vacuum in the chamber 11 is 1.0 × 10 ⁻⁴ [Pa], the metal fixing material is vaporized from the vapor deposition unit 15 by, for example, resistance heating vapor deposition. As the metal fixing material, for example, an organic material that can be deposited under a vacuum of 1.0 × 10 ⁻⁴ [Pa] and can form a complex easily by coordination with an alkali metal. Chelate compounds can be used. Examples of such organic chelate compounds include tris (8-quinolinolato) aluminum complex (Alq3), phenanthroline, bathophenanthroline, bathocuproine and the like which are host electron transport materials.

  The vaporized metal fixing material adheres to the surface 13 a of the crystal unit 13 located above the vapor deposition unit 15. Since the vapor deposition unit 15 is located on the vertical line of the crystal resonator 13 included in the film thickness monitor 12, the metal fixing material vaporized from the vapor deposition unit 15 adheres to the surface 13 a of the crystal resonator 13. Actually, the gas of the metal fixing material rising from the vapor deposition unit 15 spreads toward the stacked body S1. The partition plate 17 suppresses the gas of the metal fixing material from spreading toward the stacked body S1. Therefore, the gas of the metal fixing material adheres to the surface 13a of the crystal unit 13 without being deposited on the stacked body S1. When it is confirmed that the required amount of the metal fixing material has adhered to the surface 13a, the vapor deposition of the metal fixing material by the vapor deposition unit 15 is stopped.

  In FIG.2 (b), an alkali metal is vapor-deposited on the organic compound layer of laminated body S1. The alkali metal gas rises from the vapor deposition unit 14 located on the vertical line of the stacked body S1, and the alkali metal adheres to the organic compound layer of the stacked body S1 facing the vapor deposited unit 14. The alkali metal gas reaches the surface 13a of the crystal unit 13 and reacts with the metal fixing material deposited on the surface 13a. The alkali metal that has reacted with the metal fixing material on the surface 13a is fixed to the surface 13a without being sublimated again. Alkali metal deposited on the organic compound layer of the stacked body S1 is doped into the organic compound layer to form a metal doping layer, so that it hardly resublimates. Therefore, the film thickness of the alkali metal deposited on the organic compound layer of the stacked body S1 is equal to the film thickness of the alkali metal fixed to the surface 13a of the crystal resonator 13. The film thickness monitor 12 measures the film thickness of the alkali metal based on a table showing the correspondence between the change in the weight of the alkali metal deposited on the crystal resonator 13 and the frequency of the crystal resonator 13 with respect to the change in weight. The thickness of the alkali metal thus measured is equal to the thickness of the alkali metal of the stacked body S1. By performing vapor deposition while measuring the film thickness of the alkali metal with the film thickness monitor 12, the film thickness of the alkali metal deposited on the organic compound layer of the laminate S1 can be controlled, and the metal on the organic compound layer can be controlled. It is possible to accurately control the amount of doping. According to the vacuum deposition apparatus 10 according to the present embodiment, the thickness of the alkali metal can be accurately controlled with a simple apparatus configuration without introducing a film thickness measuring apparatus for separately measuring the thickness of the alkali metal. Can do.

(Second Embodiment)
FIG. 3 is a diagram schematically showing a vacuum evaporation apparatus according to the second embodiment.

  In FIG. 3, the vacuum vapor deposition apparatus 30 according to this embodiment includes a chamber 31, a film thickness monitor 32, vapor deposition units 34 and 35, a support unit 36, a control unit 38, a pump 39, and a temperature adjustment device 40. . The vacuum deposition apparatus 30 is different from the configuration of the vacuum deposition apparatus 10 according to the first embodiment in that a partition plate is not provided between the deposition unit 34 and the deposition unit 35. Except for the point that the partition plate is not provided, the vacuum deposition apparatus 30 has the same configuration as the vacuum deposition apparatus 10, and thus the description of the configuration of the vacuum deposition apparatus 30 is omitted.

  FIG. 4 is a diagram schematically showing the steps of the vacuum deposition method using the vacuum deposition apparatus 30 according to the second embodiment.

In FIG. 4A, the gas in the chamber 31 is exhausted by the pump 39 before the stacked body S <b> 2 is put into the chamber 31. In a state where the degree of vacuum in the chamber 31 is 1.0 × 10 ⁻⁴ [Pa], the metal fixing material is vaporized from the vapor deposition unit 35 by the resistance heating vapor deposition method. As the metal fixing material, for example, an organic material that can be deposited under a vacuum of 1.0 × 10 ⁻⁴ [Pa] and can form a complex easily by coordination with an alkali metal. Chelate compounds can be used.

  The vaporized metal fixing material adheres to the surface 33 a of the crystal resonator 33 located above the vapor deposition unit 35. Since the vapor deposition unit 35 is positioned on the vertical line of the crystal resonator 33 included in the film thickness monitor 32, the metal fixing material evaporated from the vapor deposition unit 35 adheres to the surface 33 a of the crystal resonator 33. Here, the stacked body S <b> 2 including the organic compound layer on which the alkali metal is deposited is not put into the chamber 31. Therefore, it is not necessary to provide a partition plate that inhibits the gas of the metal fixing material from reaching the stacked body S2.

  In FIG.4 (b), laminated body S2 is thrown in in the chamber 31, and an alkali metal is vapor-deposited on the organic compound layer with which laminated body S2 is provided. The alkali metal gas rises from the vapor deposition unit 34 located on the vertical line of the stacked body S2, and the vapor deposition unit 34 vaporizes the alkali metal on the organic compound layer of the stacked body S2 facing the vapor deposition unit 34. The alkali metal gas reaches the surface 33a of the crystal resonator 33 and reacts with the metal fixing material deposited on the surface 33a. The alkali metal that has reacted with the metal fixing material on the surface 33a is fixed to the surface 33a without being sublimated again. Alkali metal deposited on the organic compound layer of the stacked body S2 is doped into the organic compound layer, and therefore hardly sublimates. Therefore, the film thickness of the alkali metal deposited on the organic compound layer of the stacked body S2 is equal to the film thickness of the alkali metal fixed to the surface 33a of the crystal resonator 33. Since the alkali metal does not sublime from the surface 33a, the film thickness monitor 33 can stably measure the film thickness. A correspondence table of the change in the weight of the alkali metal deposited on the crystal unit 33 and the frequency of the crystal unit 33 with respect to the change in the weight is created in advance. Based on this correspondence table, the film thickness monitor 32 measures the film thickness of the alkali metal deposited on the surface 33 a of the crystal resonator 33. The alkali metal film thickness of the surface 33a thus measured is equal to the alkali metal film thickness deposited on the organic compound layer of the laminate S2.

  The vacuum vapor deposition apparatus 30 has the same advantages as the vacuum vapor deposition apparatus 10 with a simpler apparatus configuration than the vacuum vapor deposition apparatus 10 according to the first embodiment, and is a preferable apparatus as an organic EL element manufacturing apparatus. The

  The present invention is not limited to the above-described embodiment, and can be appropriately changed without departing from the spirit or idea of the invention which can be read from the claims and the entire specification, and a vacuum accompanying such a change. The vapor deposition apparatus and the vacuum vapor deposition method are also included in the technical scope of the present invention.

It is the figure which showed typically the structure of the vacuum evaporation system which concerns on 1st Embodiment. It is the figure which showed typically the process of the vacuum evaporation method which concerns on 1st Embodiment. It is the figure which showed typically the structure of the vacuum evaporation system which concerns on 2nd Embodiment. It is the figure which showed typically the process of the vacuum evaporation method which concerns on 2nd Embodiment.

Explanation of symbols

  Vacuum deposition apparatuses 10 and 30, deposition units 14, 15, 34 and 35, film thickness monitors 12 and 32, crystal resonators 13 and 33, partition plate 17, control units 18 and 38, temperature control apparatuses 20 and 40

Claims (6)

Metal deposition means for depositing a metal having a low boiling point temperature on the deposition target;
Before the metal is deposited on the deposition target, or when the metal is deposited, a metal fixing material for fixing the metal is deposited, and the metal is deposited on the deposition target. Measuring means for measuring the film thickness of the metal deposited on the deposition target, based on the weight change of the metal fixed to the metal fixing material on the deposition surface,
A vacuum vapor deposition apparatus comprising:   The vapor deposition inhibiting means for inhibiting the metal fixing material from being deposited on the deposition target when the metal fixing material is deposited on the deposition surface. Vacuum deposition equipment.   The vacuum deposition apparatus according to claim 1, further comprising a temperature adjusting unit that adjusts a temperature of the measuring unit when measuring a film thickness of the metal fixed to the metal fixing material. .   A metal fixing material vapor deposition means for vapor depositing the metal fixing material on the deposition surface; and a control means for controlling the operation of the metal vapor deposition means and the operation of the metal fixing material vapor deposition means. The metal vapor deposition means and the metal fixing material vapor deposition means provided in the inside are, under the control of the control means, vapor deposition of the metal on the vapor deposition target and vapor deposition of the metal fixing material on the vapor deposition surface. The vacuum vapor deposition apparatus according to claim 1, wherein the vacuum evaporation apparatus is performed before and after.   5. The vacuum deposition according to claim 4, wherein when the metal deposition unit deposits the metal on the deposition target, the metal fixing material deposition unit deposits the metal fixing material on the deposition surface. apparatus. A metal deposition process for depositing a metal having a low boiling point temperature on the deposition target;
A metal fixing material vapor deposition step for vapor-depositing a metal fixing material for immobilizing the metal on the deposition target before the deposition of the metal on the deposition target,
When the metal is deposited on the deposition target, the thickness of the metal deposited on the deposition target is determined based on the weight change of the metal fixed to the metal fixing material on the deposition target surface. Measuring process to measure,
A method for forming a thin film, comprising:

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