JP2005203248A - Vapor deposition method and vapor deposition device - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a vapor deposition method and a vapor deposition device wherein by suppressing adhesion and accumulation of vapor deposition materials in a vacuum chamber to the minimum, vapor deposition film of homogeneous film-thickness and high-purity can be formed while keeping utilization efficiency and film-forming rate of the vapor deposition materials high, and on that occasion, wherein an amorphous organic compound film having smooth surface characteristic and a multi-component vapor deposition film can be fabricated. <P>SOLUTION: In the vacuum chamber 1, the substrate 3 and the vapor deposition source 5 are opposed, and at the vapor deposition source 5, an introduction part 11 of a gas 15 and a gas flow passage 12 which penetrates the center part of the vapor deposition source 5 from the lower part to the upper part are installed, and a gas flow 10 which goes from the vapor deposition source 5 into the direction of the substrate 3 is formed, and vapor molecules of the vapor deposition material discharged from the vapor deposition source 5 along the gas flow passage 10 is brought about to the substrate 3. Furthermore, a peripheral wall of a container 5b to house the vapor deposition material 5a is installed in a protruded state, and this peripheral wall protruding part 20 is controlled in a temperature in which the vapor deposition material 5a is not accumulated, and the vapor molecules are made to function as a barrier and a guide to guide the vapor molecules toward the substrate 3. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

  The present invention relates to a vapor deposition method and a vapor deposition apparatus for producing an organic compound film or the like used for an organic EL (electroluminescence) element.

  An organic compound film used for an organic EL element constituting an organic EL display is formed by a vacuum vapor deposition method when the organic compound has a low molecular weight.

  In the vacuum vapor deposition method, a vapor deposition source and a substrate are placed facing each other in a vacuum chamber, the vapor deposition source is heated in a state where the vacuum chamber is evacuated, the vapor deposition material is evaporated or sublimated, and the generated vapor molecules are removed. A film is deposited on the surface of the substrate.

Usually, the vacuum deposition method is performed under a pressure of 10 ⁻⁷ to 10 ⁻² Pa, and the mean free path of vapor molecules at this time is about 7 × 10 ^{1 to} 7 × 10 ⁶ cm. Vapor molecules released from the air travel almost straight on with no collision with other molecules, and collide with the substrate.

  At this time, if the distance between the deposition source and the substrate is too short, a difference occurs in the number of vapor molecules flying between the central portion and the peripheral portion of the substrate, and the film thickness of the film formed on the substrate becomes non-uniform. The problem of being easy arises. On the other hand, since vapor molecules jumping out from the deposition source jump out in various directions and go straight as they are, if the distance between the deposition source and the substrate is increased, many vapor molecules do not collide with the substrate and do not contribute to film formation. As described above, the vacuum vapor deposition method conventionally used has a problem that the utilization efficiency of the vapor deposition raw material is low, and as a result, the film forming speed is also slow.

  Furthermore, since the vapor molecules that have not collided with the substrate reach the inner wall of the vacuum chamber and adhere to the inner wall of the vacuum chamber, the vapor deposition material tends to adhere to the inner wall of the chamber. There is also the problem of being easily contaminated.

  The above-mentioned contamination is particularly problematic when different materials are vacuum-deposited one after another by repeatedly using the same vacuum chamber, as in the case of forming a multilayer film made of different materials on a substrate. That is, when a new layer is formed, the previous material deposited on the inner wall of the vacuum chamber is heated and evaporated, which mixes with the newly formed deposited film and lowers the purity of the deposited film. cause. In this case, since the organic compound has a low evaporation temperature, contamination due to re-evaporation is particularly likely to occur. Accordingly, the problem of contamination is particularly important in the production of multilayer films of organic compounds used in organic EL devices and the like.

  In order to cope with these problems, a vapor deposition method called a hot wall method has been developed (see Patent Document 1 described later).

  FIG. 18 is an explanatory view showing an example of a vacuum vapor deposition apparatus to which the hot wall method is applied. In the apparatus shown in FIG. 18, an inner wall 65 is provided so as to surround a space connecting the vapor deposition source 63 and the substrate 64 placed facing each other in the vacuum chamber 61, and the inner wall 65 has a temperature at which no vapor deposition material is deposited. Has been heated.

  The high-temperature inner wall (hot wall) 65 functions as a barrier and a guide that prevents the movement of the molecules 67 of the vapor deposition material to fly in a direction other than the direction of the substrate 64 and directs the molecule 67 toward the substrate 64. The hot wall method has a double structure with a high temperature inner wall (hot wall) 65, thereby improving the utilization efficiency of the vapor deposition material and condensing the vapor deposition material on the wall surface of the vacuum chamber 61. This is a vacuum vapor deposition method that minimizes this, prevents contamination in the vacuum chamber 61, maintains a high vacuum quality, and enables formation of a high-purity vapor deposition film.

  However, in the hot wall method, it is difficult to precisely control the production of the multi-component vapor deposition film, as in the conventional vacuum vapor deposition method. In particular, like the host material and guest material of the organic EL element, the evaporation temperature, etc. It is difficult to form a film by co-evaporating a plurality of components having greatly different deposition conditions. In order to prevent the deposition material having a high evaporation temperature from adhering, it is necessary to set the temperature of the hot wall 55 to be equal to or higher than the deposition temperature of the material. This is because it becomes difficult to control the deposition rate of a material having a significantly lower value. Further, since the hot wall 65 is provided close to the substrate 64, there is also a problem that the deposited film on the substrate 64 is easily affected by the radiant heat from the hot wall 65. This is an obstacle when it is desired to keep the temperature of the deposited film below the melting point to prevent crystallization and form an amorphous film.

  On the other hand, unlike the vacuum deposition method, a low pressure organic compound vapor deposition method called LPOVPD (Low Pressure Organic Vapor Phase Deposition) method has recently been developed by Princeton University (see Patent Document 2 described later).

  The OVPD method (organic compound vapor deposition method) is an organic compound film forming method in which a reactive gas is transported to a substrate by a carrier gas, and the reactive gas is reacted on the substrate to form a thin film. When this method is used, it is expected that organic materials having remarkably different vapor pressures can be co-deposited and the amount of each component in the multi-component deposition film can be precisely controlled.

The LPOVPD method is a method in which the OVPD method is performed under a pressure lower than the atmospheric pressure, and the pressure is 1 × 10 ^{−3 to} 100 Torr (about 1.3 × 10 ⁻¹ to about 1.3 × 10 ^4). Pa), the mean free path of the reaction molecules at this time is approximately 5 × 10 ^{−5 to 5} cm.

  FIG. 19 is an explanatory diagram showing an example of a vapor deposition apparatus to which the LPOVPD method is applied. In the apparatus of FIG. 19, a carrier gas whose flow rate is appropriately controlled is supplied from the carrier gas supply system 71 to each reactant. The reactant vapor dissolved in the crucible 72 and the solvent in the bubbler 73 is taken into the carrier gas flow and sent to the reaction vessel 75 from the reaction gas inlet 74. The reaction vessel 75 has a substrate 77 whose temperature is controlled by a temperature control block 78, and the vapors of the reactants react on the substrate 77 to form a thin film.

  In the LPOVPD method, since the pressure in the apparatus is higher than that in the vacuum deposition apparatus and the mean free path of gas molecules is small, the movement of the vapor molecules of the reactant is under the control of the flow of the carrier gas. Therefore, by precisely controlling the flow rate of each carrier gas, the flow rate of the vapor of each reactant can be controlled to a predetermined size and transported onto the substrate 76 for reaction.

  However, in order to avoid the crystallization of organic compound films and the growth of crystal grains, and to form amorphous and form organic compound films with good surface properties, the increase in substrate temperature accompanying the transport of high-temperature reaction gas is suppressed as much as possible. However, the substrate temperature during the formation of the thin film must be maintained near room temperature or below the crystallization temperature.

  In the OVPD method and the LPOVPD method, film formation is performed under atmospheric pressure or a vacuum with a low degree of vacuum. The film grown under such conditions is rough and has a problem of having a non-uniform surface morphology due to vapor phase nucleation and diffusion-controlled growth processes.

JP 2002-80961 A (4th, 5th page, FIG. 1) JP-T-2001-523768 (pages 7 to 12, FIG. 1)

  In view of the above situation, the object of the present invention is to keep the utilization efficiency and deposition rate of vapor deposition raw material high while keeping the vapor deposition material adhering and depositing in the vacuum chamber to a minimum. A vapor deposition method and a vapor deposition apparatus that can form a high-purity vapor-deposited film with a simple film thickness, and at the same time, can produce an amorphized organic compound film having a smooth surface property and a multi-component co-vapor-deposited film. There is to do.

  That is, in the present invention, when forming a vapor deposition film on a substrate, the substrate and the vapor deposition source are opposed to each other, and a gas flow from a region inside the periphery of the vapor deposition source toward the substrate is formed. The present invention relates to a vapor deposition method for entraining a vapor deposition material released from the vapor deposition source in the direction of the substrate by the gas flow, and a vapor deposition apparatus used for carrying out the vapor deposition method, wherein the substrate and the vapor deposition are used. And a source provided in a vacuum chamber, and a means for forming a gas flow from a region inside the periphery of the deposition source toward the substrate.

  According to the present invention, when forming a vapor deposition film on a substrate, the substrate and the vapor deposition source are opposed to each other, and a gas flow from a region inside the periphery of the vapor deposition source toward the substrate is formed. This gas flow entrains the vapor deposition material released from the vapor deposition source in the direction of the substrate, so that a sufficient distance between the substrate and the vapor deposition source is maintained while keeping the use efficiency of the vapor deposition material and the film forming speed high. be able to. As a result, the vapor deposition film can be formed with a uniform film thickness, is less susceptible to heating by radiant heat from the vapor deposition source, and the temperature of the vapor deposition film is maintained at a temperature equal to or lower than the melting point of the vapor deposition material. Crystallization can be prevented and an amorphous organic compound film having smooth surface properties can be formed. Further, it is possible to form the high-purity vapor-deposited film by minimizing the deposition and deposition of the vapor deposition substance in the vacuum chamber and minimizing contamination in the vacuum chamber.

  Here, the gas flow forms a flow straight from the region inside the periphery of the vapor deposition source toward the substrate, and mixes with the vapor deposition material released from the vapor deposition source. The vapor deposition material is taken into its own flow and functions to efficiently entrain the vapor deposition material onto the substrate. At this time, by adjusting the gas flow rate, the uniformity of the film thickness distribution and the controllability of the film formation rate can be improved. Even if the vapor deposition material is entrained, it is sufficient to support the vapor deposition material to move straight from the vapor deposition source to the substrate in the vacuum chamber. The film can be formed at a low temperature, and the film quality is improved.

  Moreover, if the constituent component of a vapor deposition film is included in the gas, a multi-component co-deposition film can be easily formed. At that time, the component ratio can be precisely controlled by adjusting the gas flow rate.

  In the present invention, as a method for incorporating the vapor deposition material into the gas flow, the gas flow path is formed so as to penetrate the central part of the vapor deposition source from the lower part to the upper part, and the gas flow passing through the vapor deposition source. By the method of entraining the vapor deposition material, the gas flow path is formed from the peripheral part of the vapor deposition source toward the upper central part thereof, and the gas flow flowing from the peripheral part of the vapor deposition source toward the upper central part A method of entraining the vapor deposition material, or using these two together, the gas flows so as to penetrate the vapor deposition source, and the gas flows from the periphery of the vapor deposition source toward the upper central portion. A method of entraining the deposition material by a gas flow is preferable.

  In addition, it is preferable to narrow a gas outlet from the vapor deposition source. At this time, the outlet port is preferably cylindrical, and the cylindrical portion of the outlet port is preferably directed upward and / or downward. By narrowing the gas outlet, a strong gas flow toward the substrate can be generated. Further, when the outlet port has a cylindrical shape, the gas flow can be directed in a direction along the inner wall surface of the cylindrical portion, so that the direction of the cylindrical portion is directed from the vapor deposition source to the substrate. If fixed, the direction of gas flow can be directed from the vapor deposition source to the substrate.

  In addition, as a specific method of forming the gas flow path from the peripheral portion of the vapor deposition source toward the upper central portion thereof, an outer wall surrounding the outer periphery of the vapor deposition source is provided, and the outer wall and the vapor deposition source It is preferable to introduce the gas in between.

  Further, a buffer space for the gas may be provided below the vapor deposition source, the gas may be temporarily stored in the buffer space, and the gas may be supplied from the buffer space to the vapor deposition source. By providing the buffer space, it is possible to supply a stable gas flow with little disturbance.

  Further, if the gas flow is used only as a wall made of gas, an inert gas may be used as the gas. Examples of the inert gas include nitrogen, argon, helium, krypton, and xenon, but are not limited thereto, and are inert and stable with respect to the vapor deposition material used for forming the vapor deposition film. Any material can be used.

Moreover, if the gas containing the component which forms the said vapor deposition film is used as said gas, the multi-component co-vapor deposition film which consists of the said vapor deposition substance and the component from this gas can be formed. Examples of such gases include inert gases such as nitrogen, argon, helium, krypton, and xenon, or gases that are inert and stable with respect to the deposition material used for forming the deposited film, and organic EL elements. A mixed gas with an evaporation component such as tris (8-hydroxyquinolinato) aluminum (III) (Alq ₃ ) as a host material or coumarin as a guest material can be used.

  Further, as the gas, an inert gas and a gas containing a component that forms the vapor deposition film are alternately switched and supplied, and a single component vapor deposition film and a multi-component co-vapor deposition film are alternately formed. it can.

  Further, the vapor deposition source and the container for containing the vapor deposition material constitute the vapor deposition source, the peripheral wall of the container protrudes toward the base, and between the protruding end of the peripheral wall and the base It is preferable to provide a predetermined distance. At this time, the peripheral wall is preferably heated. The peripheral wall functions as a barrier and a guide for guiding vapor molecules of the vapor deposition material toward the substrate, as in the hot wall of Patent Document 1 described above, and the vapor deposition material adheres if heated to a high temperature. There is no accumulation. However, unlike the hot wall formed up to the vicinity of the base body, the protruding end portion of the peripheral wall is not formed closer to the base body than the predetermined distance, and the predetermined distance is set appropriately. Thereby, it is possible to prevent the vapor deposition film formed on the substrate from being adversely affected by radiant heat from the peripheral wall.

  In addition to the gas flow, a second gas introduction portion is provided around the vapor deposition source to form a second gas flow from the circumference of the vapor deposition source toward the substrate. The direction of the gas flow may be regulated to the direction of the substrate by the gas flow of 2. Here, the second gas flow prevents the movement of the molecules of the vapor deposition material that are going to travel in a direction other than the direction of the substrate by molecular collision, and causes a wall (barrier and gas) to be directed toward the substrate. It functions as a guide.

  The second gas introduction section provided around the vapor deposition source may be formed in a region sandwiched between the vapor deposition source and a guide provided around the vapor deposition source. According to this structure, the flow of the second gas surrounding the space from the vapor deposition source to the substrate can be formed with a simple configuration.

  Alternatively, the second gas may be supplied to a buffer space provided below the vapor deposition source, and the second gas may be led out from the buffer space along the peripheral wall of the vapor deposition source. By providing the buffer space, it is possible to form a stable second gas flow with little disturbance.

  In addition, the gas or the second gas supply unit may be provided at one or a plurality of locations with respect to the gas or the second gas introduction unit, respectively. The gas supply unit may be opened in a porous or slit shape with respect to the gas introduction unit along a peripheral wall of the vapor deposition source. When the supply unit is provided in many places, or the opening is formed continuously like a slit, the gas flow or the second gas is more uniform in the circumferential direction of the vapor deposition source. It is thought that a flow is easily formed. However, the shape of the gas supply unit is not limited to these.

The vapor deposition film formed in the present invention is not particularly limited, but it is preferable to form a thin film of an organic compound. For example, in the case of forming an organic EL element, tris (8-hydroxyquinolinato) aluminum (III) (Alq ₃ ), quinacridone, rubrene, N, N′-bis (3-methylphenyl) -1,1′- Biphenyl-4,4′-diamine (TPD), 4,4′-bis (N-naphthyl-N-phenylamino) biphenyl (α-NPD), bathophenanthroline, bathocuproine and oxadiazole.

  Next, a preferred embodiment of the present invention will be described in detail with reference to the drawings.

Embodiment 1
FIG. 1 is an explanatory diagram (a) showing a configuration of a vapor deposition apparatus (Example 1) based on Embodiment 1 of the present invention, and a vapor deposition source 5 viewed from the position of the line 1b-1b shown in FIG. 1 (a). And a plan view (b) of the peripheral device.

The vacuum chamber 1 is composed of an airtight hollow container provided with an exhaust system 2 composed of a vacuum pump, an exhaust valve, a trap, etc. (not shown), and the shape thereof is not limited. The exhaust system 2 is configured so that the vacuum chamber 1 can be exhausted to a high vacuum state of about 1 × 10 ⁻⁵ Pa or more.

  As a material of the substrate 3 which is a substrate on which the deposited film is formed, any material such as glass, ceramics, metal or resin can be used depending on the application.

  The substrate support 4 is disposed at the upper center position of the vacuum chamber 1 and has a lower surface formed in a planar shape, and is configured to hold the substrate 3 on this surface. In order to securely hold the substrate 3 on the lower surface of the substrate support 4, an electrostatic adsorption method in which static electricity is induced and held on the lower surface is adopted, or the edge of the substrate 3 is mechanically moved by an L-shaped member. Alternatively, a method of holding it may be adopted.

  The substrate support 4 is provided with a substrate heating heater and a cooling device for heating and / or cooling the substrate 3 to a predetermined temperature. For example, this heater is a resistance heating type, and the cooling device is water-cooled. Of the formula. Although not shown, the chamber 1 has a temperature measuring means for measuring the temperatures of the substrate 3 and the substrate support 4 and the power supplied to the substrate heating heater is adjusted according to a signal from the temperature measuring means. A controller and a power source for controlling the temperature and flow rate of the cooling refrigerant and a power source, and a fixing means for fixing the substrate support 4 to the chamber 1 are provided.

  A vapor deposition source 5 is placed at the center of the lower portion of the vacuum chamber 1 so as to face the substrate 3. The vapor deposition source 5 includes a vapor deposition material 5a and a container 5b that accommodates the vapor deposition material 5a. Below the vapor deposition source 5, an evaporation source heating unit 6 that controls the temperature of the vapor deposition material 5a is provided. The evaporation source heating means 6 includes, for example, a resistance heating type evaporation source heating heater or heating lamp, a temperature measuring means for measuring the temperature of the vapor deposition material 5a, and an evaporation source heating heater according to a signal from the temperature measuring means. Alternatively, it includes a controller and a power source for adjusting the power supplied to the heating lamp. FIG. 1 shows an example in which the shape of the container 5b is a cylindrical shape, but the shape and material of the container 5b are not particularly limited, and are appropriately selected according to the vapor deposition material 5a.

Although it does not specifically limit as the vapor deposition substance 5a, For example, in the case of forming an organic EL element, tris (8-hydroxyquinolinato) aluminum (III) (Alq ₃ ), quinacridone, rubrene, N, N '-Bis (3-methylphenyl) -1,1'-biphenyl-4,4'-diamine (TPD), 4,4'-bis (N-naphthyl-N-phenylamino) biphenyl (α-NPD), Such as bathophenanthroline, bathocuproine and oxadiazole.

  Alternatively, an organic semiconductor layer can be formed using an organic compound such as pentacene, oligothiophene, a phthalocyanine metal complex, or a substituted derivative thereof as the vapor deposition material 5a.

  Above the vapor deposition source 5, a shutter 7 for controlling the vapor deposition operation is provided. When the shutter 7 is closed, the movement of the vapor of the vapor deposition material heated and released by the vapor deposition source 5 into the vacuum chamber 1 is suppressed.

  In the present embodiment, the vapor deposition source 5 is provided with an introduction portion 11 for the gas 15. The gas introduction part 11 is formed so that the gas flow path 12 penetrates the central part of the vapor deposition source 5 from the lower part to the upper part. According to this structure, the gas flow 10 flowing through the vapor deposition source 5 and taking in the vapor deposition material 5a can be formed with a simple configuration. In the apparatus of FIG. 1, one gas supply unit 13 is provided for the gas introduction unit 11.

  Further, the peripheral wall of the vapor deposition material container 5 b is provided so as to protrude toward the substrate 3. The temperature of the peripheral wall protruding portion 20 is controlled independently of the vapor deposition material 5a by the built-in heater and temperature measuring means, and functions in the same manner as the hot wall disclosed in Patent Document 1. In other words, the peripheral wall protruding portion 20 functions as a barrier and a guide that prevents the vapor molecules of the vapor deposition material 5a from flying in a direction other than the direction of the substrate 3 and moves toward the direction of the substrate 3. Since it is kept at a high temperature by heating, the vapor deposition material 5a does not adhere to the peripheral wall protruding portion 20 and deposit.

However, the protruding end 20c of the peripheral wall protruding portion 20 is not formed closer to the substrate 3 than a predetermined distance. As shown in FIG. 1A, the distance from the surface of the vapor deposition material 5a in the container 5b to the protruding end 20c is set as h ₁ , and the distance from the protruding end 20c to the substrate 3 is set as h _2. To do. If h ₁ / (h ₁ + h ₂ ) is too small, the effect of the peripheral wall protruding portion 20 as a barrier and guide cannot be obtained sufficiently. On the other hand, if h ₂ is too small, there is an adverse effect such that the deposited film formed on the substrate 3 is heated to the melting point or higher by radiant heat from the peripheral wall protruding portion 20 and crystallized. Therefore, it is necessary to set h ₁ and h ₂ appropriately. In the present embodiment, by setting h ₁ to ₁ to 30 cm and h ₂ to ₂ to 30 cm, vapor deposition by radiant heat from the peripheral wall protruding portion 20 while sufficiently exerting the effect of the peripheral wall protruding portion 20 as a barrier and guide. The adverse effect on the membrane can be avoided.

  Further, in the present embodiment, a part 20a of the peripheral wall protruding portion 20 in the vicinity of the protruding end 20c is provided so that the diameter of the peripheral wall is reduced, and the cross-sectional area of the gas outlet 8 is made of the vapor deposition material 5a in the vapor deposition source 5 It is narrower than the surface area. By narrowing down the gas outlet 8, the gas flow rate at the gas outlet 8 can be increased, and a strong gas flow 10 toward the substrate 3 can be generated.

  Next, the process of forming a vapor deposition film using the vapor deposition apparatus shown in FIG. 1 is demonstrated.

  First, after the substrate 3 and the vapor deposition material 5a are arranged at predetermined positions, the vacuum chamber 1 is evacuated to a predetermined vacuum level. At this time, the shutter 7 is closed.

  Next, power is supplied to a temperature control device such as a substrate heating heater and / or cooling device for the substrate support 4, a vapor deposition source heating heater or a heating lamp for the vapor deposition source heating means 6, and the substrate 3, the vapor deposition source 5 and the peripheral wall. The protruding portions 20 are each adjusted to a predetermined temperature.

  Next, when the temperature of the substrate 3, the vapor deposition source 5 and the peripheral wall protruding portion 20 reaches a predetermined temperature, the shutter 7 is opened, and vapor molecules of the vapor deposition material 5 a are deposited on the substrate 3. At this time, the gas 15 is supplied from the gas supply pipe 14 to the gas inlet 11.

  The gas 15 introduced into the gas introduction part 11 takes in vapor molecules released from the surface of the vapor deposition material 5 a while flowing from the gas introduction part 11 to the gas outlet 8, and flows out from the gas outlet 8. According to the pressure difference in the vacuum chamber 1, a gas flow 10 traveling straight from the gas outlet 8 toward the substrate 3 is formed, and vapor molecules are efficiently entrained on the substrate 3. At this time, since the peripheral wall diameter reducing portion 20a is provided and the cross-sectional area of the gas outlet 8 is narrowed, the flow velocity of the gas at the gas outlet 8 is increased, a strong gas flow 10 is formed, and the vapor molecules are formed on the substrate. The efficiency of taking 3 up is increased.

The moving direction 9 of the vapor molecules of the vapor deposition material released from the vapor deposition source 5 is regulated so as to be directed toward the substrate 3 by the inner wall of the peripheral wall protruding portion 20 and the gas flow 10. That is, from the surface of the vapor deposition material 5 a to the height h ₁ cm, the movement of the vapor molecules in the direction other than the direction of the substrate 3 is reflected by the inner wall of the peripheral wall protruding portion 20 and is restricted to the direction of the substrate 3. Is done. The vapor molecules are taken into the gas flow 10 in the space between the gas inlet 11 and the gas outlet 8, pushed out from the gas outlet 8 into the vacuum chamber 1, and flowed into the vacuum chamber 1. Is entrained in a gas flow 10 traveling straight in the direction of the substrate 3 and efficiently carried onto the substrate 3. Even when the gas flow 10 is a straight upward flow as shown by the arrows in FIG. 1A, it actually flows while spreading in the horizontal direction of the figure, so it is uniform with the vapor molecules of the vapor deposition material. It is considered that they mix and reach the vicinity of the substrate 3.

  Thus, since the movement 9 of the vapor molecules of the vapor deposition material is controlled by the gas flow 10, the uniformity of the film thickness distribution and the controllability of the film forming speed can be improved by adjusting the gas flow rate. Can do. At this time, even if the vapor molecules are entrained, it is sufficient to support the vapor molecules to move straightly from the gas outlet 8 to the substrate 3 in the vacuum chamber 1, so that compared with the LPOVPD method. A film can be formed under a high degree of vacuum, and the film quality is improved.

  Further, in the normal vacuum vapor deposition method, when the peripheral wall diameter reducing portion 20a is provided, the number of vapor molecules arriving from the vapor deposition source 5 to the substrate 3 is immediately reduced due to the reduction of the opening area, resulting in a decrease in the film formation rate. However, in the present embodiment, the vapor molecules are taken into the gas flow 10 in the space between the gas inlet 11 and the gas outlet 8 and pushed out into the vacuum chamber 1. Therefore, even if the peripheral wall diameter reducing portion 20a is provided, the film forming speed is not immediately reduced.

  According to the present embodiment, by using the gas flow 10 and the peripheral wall protruding portion 20 in combination, the flight direction of the vapor molecules is guided toward the substrate 3, so that the utilization efficiency of the deposition material and the film formation speed are kept high. A sufficient distance between the substrate 3 and the vapor deposition source 5 can be taken, and the vapor deposition film can be formed with a uniform film thickness. In addition, it is possible to form a high-purity vapor deposition film by minimizing the deposition and deposition of a vapor deposition substance in the vacuum chamber 1 and minimizing contamination in the vacuum chamber 1.

  As in the hot wall method of Patent Document 1, if it is attempted to restrict the flight direction of vapor molecules only with the hot wall, it is necessary to provide the hot wall up to the vicinity of the substrate 3, and the deposited film on the substrate 3 is formed. This creates a new problem of being easily affected by radiant heat from the hot wall. According to the present embodiment, it is not necessary to provide a hot wall in the vicinity of the substrate 3 by using the gas flow 10 together, and there is no fear that the deposited film is heated by the radiant heat from the hot wall. Therefore, the vapor deposition film can be easily maintained at a temperature lower than the melting point of the vapor deposition material to prevent crystallization, and an amorphous organic compound film having smooth surface properties can be formed.

  If the gas flow 10 is used only as a transport medium for entraining vapor molecules, an inert gas is supplied as the gas 15. Examples of the inert gas include nitrogen, argon, helium, krypton, and xenon. However, the inert gas is not limited thereto, and is inert and stable with respect to the vapor deposition material 5a used for forming the vapor deposition film. Any substance can be used. Note that the temperature of the gas stream 10 is maintained at a high temperature such that vapor molecules of the vapor deposition material are not condensed in the gas phase.

In addition, if the gas 15 contains the constituent components of the vapor deposition film, a multi-component co-deposition film composed of the vapor deposition material 5a and the constituent components from the gas can be easily formed. At this time, the component ratio can be precisely controlled by adjusting the gas flow rate. Examples of such gases include inert gases such as nitrogen, argon, helium, krypton, and xenon, or gases that are inert and stable with respect to the deposition material used for forming the deposited film, and organic EL elements. A mixed gas with an evaporation component such as tris (8-hydroxyquinolinato) aluminum (III) (Alq ₃ ) as a host material or coumarin as a guest material can be used.

  Further, as the gas 15, an inert gas and a gas containing a component for forming a vapor deposition film are alternately switched and supplied, and a single component vapor deposition film and a multi-component co-vapor deposition film can be alternately formed. .

  2 and 3 are a cross-sectional view (a) and a plan view (b) showing another example of the vapor deposition source and its peripheral device based on the present embodiment.

  The vapor deposition source of Example 2 shown in FIG. 2 is an example in which a cylindrical portion 20b is provided at the tip of the peripheral wall diameter reducing portion 20a of the vapor deposition source 5 of Example 1 shown in FIG. When the cylindrical portion 20b is provided at the gas outlet 8, the gas flow 10 can be directed in a direction along the inner wall surface of the cylindrical portion 20b. Therefore, the direction of the cylindrical portion 20b is directed toward the substrate 3. If so, the direction of the gas flow 10 can be directed from the vapor deposition source 5 to the substrate 3, the utilization efficiency of the vapor deposition material 5 a is increased, the film formation speed is improved, and contamination in the vacuum chamber 1 is suppressed. be able to.

  In the vapor deposition source of Example 3 shown in FIG. 3 (1), a buffer space 16 of gas 15 is provided below the vapor deposition source 5 of Example 1, gas 15 is temporarily stored in the buffer space 16, and vapor deposition is performed from the buffer space 16. In this example, the gas 15 is supplied to the source 5. By providing the buffer space 16, it is possible to supply a stable flow of the gas 15 with less disturbance. The vapor deposition source of Example 4 shown in FIG. 3B is an example in which a buffer space 16 of gas 15 is provided below the vapor deposition source 5 having the cylindrical portion 20b of Example 2, and the effect of the buffer space 16 in this case Is the same as above.

  These vapor deposition sources are used by being fixed to a vapor deposition apparatus similar to that shown in FIG. 1, but when the buffer space 16 is provided, the vapor deposition source heating means is provided at the lower part or the side part of the vapor deposition source. It is done.

Embodiment 2
FIG. 4A is a cross-sectional view (a) and a plan view (b) showing the vapor deposition source 25 of Example 5 and its peripheral devices based on Embodiment 2 of the present invention.

  In the apparatus of Example 5, the outer wall 17 and the upper lid 18 surrounding the outer periphery of the vapor deposition source 25 are provided, and the introduction portion 21 of the gas 15 is formed in a space region surrounded by the vapor deposition source 25, the outer wall 17, and the upper lid 18. . The gas flow path 22 passes from the gas introduction part 21 through the peripheral part of the vapor deposition source 25 to the upper central part of the vapor deposition source 25 and enters the vacuum chamber 1 from the outlet 8B provided in the central part of the upper lid 18. Is formed. According to this structure, the gas that flows along the surface of the vapor deposition material 5a between the gas introduction part 21 and the gas outlet 8B, efficiently takes in the vapor molecules released from the surface of the vapor deposition material 5a, and entrains the gas. The flow can be formed with a simple configuration. In the apparatus of FIG. 4, one gas supply unit 23 is provided for the gas introduction unit 21, but gas supply units may be provided at a plurality of locations as will be described later.

  The outer wall 17 and the upper lid 18 are kept at a predetermined temperature by a heater (not shown), a temperature measuring means, and a controller and a power source that adjust power supplied to the substrate heating heater in accordance with a signal from the temperature measuring means. Therefore, the vapor deposition material 5a does not adhere and deposit. Accordingly, the outer wall 17 and the upper lid 18 can also be regarded as part of a hot wall that guides vapor molecules in the direction of the substrate 3, similarly to the peripheral wall protruding portion 20 connected to the vapor deposition source 25.

  However, the upper lid 18 is not disposed closer to the substrate 3 than a predetermined distance, and the vapor deposition film formed on the substrate 3 is heated to the melting point or more by the radiant heat from the upper lid 18 or the outer wall 17 to cause a crystal. It is possible to prevent adverse effects such as conversion.

  The vapor deposition source 25 and its peripheral devices of Example 5 shown in FIG. 4A are fixed and used in the same vacuum chamber 1 as shown in FIG. Hereinafter, the process of forming a vapor deposition film using the vapor deposition source 25 and its peripheral devices and the characteristics thereof will be described with emphasis on the differences from the first embodiment.

  First, after the substrate 3 and the vapor deposition material 5a are arranged at predetermined positions, the vacuum chamber 1 is evacuated to a predetermined vacuum level. At this time, the shutter 7 is placed at the position of the virtual line and closed.

  Next, each heater is energized, such as a substrate heating heater of the substrate support 4 and a vapor deposition source heating heater of the vapor deposition source heating means 6, and the substrate 3, vapor deposition source 25, peripheral wall protruding portion 20, outer wall 17 and upper lid 18. Each is heated to a predetermined temperature.

  Next, when the temperature of the substrate 3, the vapor deposition source 25, the peripheral wall protruding portion 20, the outer wall 17 and the upper lid 18 reaches a predetermined temperature, the shutter 7 is opened, and vapor of the vapor deposition material 5 a is deposited on the substrate 3. At this time, the gas 15 is supplied from the gas supply pipe 14 to the gas introduction part 21.

  While the gas 15 introduced into the gas introduction unit 21 flows from the gas introduction unit 21 to the gas outlet 8B, it takes in vapor molecules released from the surface of the vapor deposition material 5a. After flowing out from the gas outlet 8B, according to the pressure difference in the vacuum chamber 1, a flow 10 of gas that goes straight from the gas outlet 8B toward the substrate 3 is formed, and vapor molecules are efficiently entrained onto the substrate 3. To do. At this time, since the gas flow path 22 in the vapor deposition source 25 is formed so as to be along the surface of the vapor deposition material 5a, the efficiency of taking in the vapor molecules released from the surface of the vapor deposition material 5a is the apparatus of the first embodiment. There are high advantages compared to.

  Further, since the vapor molecules are taken in by the horizontal gas flow, the vapor molecules in the vertical gas flow (the gas flow between the gas inlet 11 and the gas outlet 8 in FIG. 1). Compared with Embodiment 1 in which the uptake is performed, the height in the vertical direction can be reduced, and the whole can be made compact.

  In addition, since there is no fear that the gas 15 passes through the vapor deposition source 25 without being mixed with vapor molecules, the diameter of the opening of the gas outlet 8B is reduced to the limit necessary to ensure the gas flow rate. Can do. For this reason, the gas flow 10 having a high flow rate can be formed in the vacuum chamber 1, and the efficiency of entraining vapor molecules to the substrate 3 can be increased.

  The present embodiment has other features similar to those of the first embodiment. That is, by using the gas flow 10 and the outer wall 17, the upper lid 18, and the peripheral wall protruding portion 20 together, the flight direction of the vapor molecules is guided toward the substrate 3. 3 and the vapor deposition source 25 can be sufficiently spaced to form a vapor deposition film with a uniform thickness. Further, it is possible to form a high-purity vapor deposition film by minimizing the deposition and deposition of the vapor deposition material 5a in the vacuum chamber 1 and minimizing contamination in the vacuum chamber 1.

  Further, there is no need to provide a hot wall in the vicinity of the substrate 3, there is no concern that the deposited film is heated by the radiant heat from the hot wall, and the substrate temperature is kept below the melting point of the deposited material to prevent crystallization and smooth An amorphized organic compound film having excellent surface properties can be formed.

Moreover, if the component of a vapor deposition film is included in the gas 15, a multi-component co-deposition film can be easily formed. At this time, the component ratio can be precisely controlled by adjusting the gas flow rate. Examples of such gases include inert gases such as nitrogen, argon, helium, krypton, and xenon, or gases that are inert and stable with respect to the deposition material used for forming the deposited film, and organic EL elements. Examples thereof include a mixed gas with an evaporation component such as tris (8-hydroxyquinolinato) aluminum (III) (Alq ₃ ) as a host material or coumarin as a guest material. Further, as the gas 15, an inert gas and a gas containing a component for forming a vapor deposition film are alternately switched and supplied, and a single component vapor deposition film and a multi-component co-vapor deposition film can be alternately formed. .

  FIG. 4B is a cross-sectional view (a) and a plan view (b) showing another example (Example 6) of the vapor deposition source and its peripheral device based on the present embodiment.

  The apparatus of Example 6 is an example in which a cylindrical portion 19 is provided below the outlet 8B of the apparatus of Example 5 shown in FIG. If the cylindrical part 19 is provided in the lower part of the gas outlet 8B, the gas flow can be directed in a direction along the inner wall surface of the cylindrical part 19, so that the direction of the cylindrical part 19 is fixed so as to face the substrate 3. If so, the direction of the gas flow 10 can be directed from the vapor deposition source 25 toward the substrate 3, the utilization efficiency of the vapor deposition material 5 a can be increased, and contamination in the vacuum chamber 1 can be suppressed. The direction of the cylindrical portion 19 may be provided downward as shown in the figure, or may be provided in the upper direction or both the upper and lower directions although illustration is omitted (the same applies to Examples 7 to 10 below).

  The cylindrical portion 19 provided below has an effect of suppressing the flow of gas that flows out without flowing near the surface of the vapor deposition material 5a, and improving the uniformity of the concentration of vapor molecules contained in the outflow gas. .

  5 and 6 are a cross-sectional view (a) and a plan view (b) showing another example of the vapor deposition source and its peripheral device based on the present embodiment.

  The apparatus of Example 7 shown in FIG. 5 (1) is the apparatus of Example 6, in which the bottom of the vapor deposition container 25b at a position facing the tubular part 19 is raised and sandwiched between the tubular part 19 and the raised part 26. This is an example in which a flow path is formed so that gas flows through a gap. In the apparatus of Example 6, since the gas flows through the gap sandwiched between the cylindrical portion 19 and the surface of the vapor deposition material 5a, the size of the void depends on the amount of the vapor deposition material 5a, and the resistance that the gas receives from the void is vapor deposition. It varies depending on the amount of the substance 5a. On the other hand, in the apparatus of Example 7, since the size of the void does not depend on the amount of the vapor deposition material 5a, the resistance that the gas receives from the void is constant, and the gas flow rate is not affected by the amount of the vapor deposition material 5a. There is.

  The apparatus of Example 8 shown in FIG. 5B is obtained by adding a gas flow path 12 that penetrates the central portion of the vapor deposition source 25 from the lower part to the upper part to the apparatus of Example 7. According to this structure, the gas flow rate can be increased without changing the flow rate of vapor molecules of the vapor deposition material 5a, a strong gas flow 10 is formed in the vacuum chamber 1, and the utilization efficiency of the vapor deposition material 5a is increased. Contamination in the vacuum chamber 1 can be suppressed.

  The apparatus of Example 9 shown in FIG. 6 (1) has a gas flow path 12 penetrating from the lower part to the upper part of the center of the vapor deposition source 25 as in the apparatus of Example 8, but the gas flowing through the flow path 12 15B is configured to be supplied from a gas supply pipe 14 different from the gas 15 flowing through the flow path 22. According to this structure, the flow rate of the gas 15B flowing through the flow channel 12 can be adjusted independently of the flow rate of the gas 15 flowing through the flow channel 22, and the vapor molecules contained in the gas flowing out from the gas outlet 8B can be adjusted. The flow rate and concentration can be controlled to desired values.

  Further, the gas 15B flowing through the flow path 12 and the gas 15 flowing through the flow path 22 can be different types of gases. For example, one gas is used as a gas containing the constituent components of the vapor deposition film, and multi-component co-deposition is performed. A film can also be formed. At this time, the component ratio of the multi-component co-deposited film can be precisely controlled by adjusting the gas flow rates of the gas 15 and the gas 15B.

  In the apparatus of Example 10 shown in FIG. 6 (2), a buffer space 27 for the gas 15 is provided below the vapor deposition source 25 of the apparatus of Example 8, and the gas 15 is temporarily stored in the buffer space 27. In this example, the gas 15 is supplied to the vapor deposition source 25. By providing the buffer space 27, a stable flow of the gas 15 with less disturbance can be supplied to the vapor deposition source 25.

  FIG. 7 is a cross-sectional view (a) and a plan view (b) showing another shape of the gas supply unit 13 based on the present embodiment.

  FIG. 7 (1) is an example in which two gas supply units 23 are provided in the gas introduction unit 21. In order to supply a gas flow that is uniform in the circumferential direction to the vapor deposition source 25, two or more gas supply units 23 are arranged in the gas introduction unit 21 at equal intervals as in this example. It is considered good. However, even if the amount is too large, the effect is not improved as the structure becomes complicated.

  7 (2) and 7 (3), instead of providing the supply section 23 at a large number of locations, the gas supply pipe 24 has a porous shape having a large number of holes (openings) 28 (FIG. 7 (2)). ) Or a shape having a continuous slit-like opening 29 (FIG. 7 (3)).

Embodiment 3
FIG. 8: is sectional drawing (a) and the top view (b) which show the vapor deposition source of Example 11 based on Embodiment 3 of this invention, and its peripheral device.

  In the apparatus of Example 11, the introduction part 31 of the second gas 35 is provided around the vapor deposition source 5 of Example 1 shown in FIG. The gas introduction part 31 is formed in a region sandwiched between the vapor deposition source 5 and a guide 32 provided around the vapor deposition source 5. According to this structure, the second gas flow 36 surrounding the gas flow 10 on its side surface can be formed with a simple configuration. In the apparatus of FIG. 8, one gas supply unit 33 is provided for the gas introduction unit 31.

  The apparatus of Example 11 shown in FIG. 8 is used by being fixed in a vacuum chamber 1 similar to that shown in FIG. Hereinafter, the process of forming a vapor deposition film using the apparatus of Example 11 and the features thereof will be described with emphasis on the differences from the first embodiment.

  First, after the substrate 3 and the vapor deposition material 5a are arranged at predetermined positions, the vacuum chamber 1 is evacuated to a predetermined vacuum level. At this time, the shutter 7 is placed at the position of the virtual line and closed.

  Next, each heater is energized, such as a heater for heating the substrate of the substrate support 4 and a heater for heating the evaporation source of the evaporation source heating means 6, and the substrate 3, the evaporation source 5, and the peripheral wall protruding portion 20 are respectively set to predetermined temperatures. Heat to.

  Next, when the temperature of the substrate 3, the vapor deposition source 5 and the peripheral wall protruding portion 20 reaches a predetermined temperature, the shutter 7 is opened, and vapor of the vapor deposition material 5 a is deposited on the substrate 3. At this time, the gas 15 is supplied from the gas supply pipe 14 to the gas introduction unit 11, and the gas introduction unit 31 sandwiched between the vapor deposition source 5 and the guide 32 provided around the vapor deposition source 5. A second gas 35 is supplied from the gas supply pipe 34.

  As described above in the first embodiment, the gas 15 introduced into the gas introduction unit 11 takes in the vapor molecules released from the surface of the vapor deposition material 5 a while flowing from the gas introduction unit 11 to the gas outlet 8, After flowing out from the gas outlet 8, a gas flow 10 that goes straight from the gas outlet 8 toward the substrate 3 is formed according to the pressure difference in the vacuum chamber 1, and vapor molecules are efficiently entrained on the substrate 3. To do.

  On the other hand, the second gas introduced into the gas introduction part 31 forms a second gas flow 36 from the periphery of the vapor deposition source 5 toward the substrate 3 according to the pressure difference in the vacuum chamber 1. At this time, the second gas flow 36 is directed in the direction along the two wall surfaces sandwiching the gas introduction part 31, the outer wall of the peripheral wall protruding portion 20 of the vapor deposition source 5, and the inner wall surface of the guide 32. Therefore, for example, when these surfaces are formed in the vertical direction in the figure as shown in FIG. 8, the second gas flow 36 is also a straight upward flow as shown by the arrows, The gas flow 10 is formed so as to surround the side surface.

  As described above in the first embodiment, the movement direction 9 of the vapor molecules of the vapor deposition material emitted from the vapor deposition source 5 is directed toward the substrate 3 mainly by the inner wall of the peripheral wall protruding portion 20 and the gas flow 10. Regulated by That is, in the vapor deposition source 5, the movement of the vapor molecules in the direction other than the direction of the substrate 3 is reflected by the inner wall of the peripheral wall protruding portion 20 and is regulated so as to go toward the substrate 3. The vapor molecules are taken into the gas flow 10 in the space between the gas inlet 11 and the gas outlet 8, pushed out from the gas outlet 8 into the vacuum chamber 1, and flowed into the vacuum chamber 1. Is entrained in a gas flow 10 traveling straight in the direction of the substrate 3 and efficiently carried onto the substrate 3.

  However, even when the gas flow 10 is a straight upward flow as shown by the arrows in FIG. 8, the gas flow actually flows in the horizontal direction of the figure, so that the vapor molecules of the vapor deposition material also move in the horizontal direction. It is thought that it flows while spreading. The vapor molecule flow 37 that tends to spread in the left-right direction is preferable for forming a uniform vapor deposition film on the substrate 3, but if it is excessive, the loss of the vapor deposition material 5a increases. The use efficiency of the vapor deposition material 5a is reduced, and the film quality is deteriorated due to contamination of the vacuum chamber 1.

  In the present embodiment, since the second gas flow 36 is formed so as to surround the gas flow 10 on the side surface, the vapor molecules excessively spread in the left-right direction and deviate from the direction toward the substrate 3. The flow 37 is restricted to go toward the substrate 3. That is, the second gas flow 36 functions as a wall (barrier and guide) by gas that prevents the movement of vapor molecules that are going to travel in directions other than the direction of the substrate 3 by molecular collision and directs them toward the direction of the substrate 3. To do.

  As described above, in this embodiment, the movement 9 of the vapor molecules of the vapor deposition material is doubly controlled by the gas flow 10 and the second gas flow 36. While keeping the film speed high, a sufficient distance between the substrate 3 and the vapor deposition source 5 can be taken, and the vapor deposition film can be formed with a uniform film thickness. In addition, it is possible to form a high-purity vapor deposition film by minimizing the deposition and deposition of a vapor deposition substance in the vacuum chamber 1 and minimizing contamination in the vacuum chamber 1. Further, by adjusting the respective gas flow rates, the uniformity of the film thickness distribution and the controllability of the film formation rate can be further improved.

Further, by using the second gas flow 36 in combination, it is possible to form a film under a higher degree of vacuum than in the case of the gas flow 10 alone, and the film quality is improved. For example, in order for the second gas stream 36 to function as a wall, the average in the second gas stream 36 is such that the second gas stream 36 does not pass vapor molecules and can be reflected by molecular collisions. The free process may be several cm or less. Since the degree of vacuum corresponding to this is about 10 ⁻¹ Pa, the film can be formed under a higher degree of vacuum than the LPOVPD method.

  In addition, it goes without saying that the present embodiment has the same characteristics as those of the first embodiment. That is, there is no need to provide a hot wall in the vicinity of the substrate 3, there is no concern that the deposited film is heated by the radiant heat from the hot wall, and the substrate temperature is kept below the melting point of the deposited material to prevent crystallization and smooth An amorphized organic compound film having excellent surface properties can be formed.

Moreover, if the component of a vapor deposition film is included in the gas 15, a multi-component co-deposition film can be easily formed. At this time, the component ratio can be precisely controlled by adjusting the gas flow rate. Examples of such gases include inert gases such as nitrogen, argon, helium, krypton, and xenon, or gases that are inert and stable with respect to the deposition material used for forming the deposited film, and organic EL elements. A mixed gas with an evaporation component such as tris (8-hydroxyquinolinato) aluminum (III) (Alq ₃ ) as a host material or coumarin as a guest material can be used. Further, as the gas 15, an inert gas and a gas containing a component for forming a vapor deposition film are alternately switched and supplied, and a single component vapor deposition film and a multi-component co-vapor deposition film can be alternately formed. .

  If the second gas stream 36 is used only as a wall by the gas 35, an inert gas is supplied as the gas 35. Examples of the inert gas include nitrogen, argon, helium, krypton, and xenon. However, the inert gas is not limited thereto, and is inert and stable with respect to the vapor deposition material 5a used for forming the vapor deposition film. Any substance can be used. For example, the larger the diameter of the molecule and the larger the mass of the molecule, the higher the effect as a wall. Therefore, tetrafluoromethane, carbon tetrachloride and the like are suitable as an inert gas if usable.

In addition, if the gas 35 contains a constituent component of the vapor deposition film, a multi-component co-deposition film can be easily formed. At this time, the component ratio can be precisely controlled by adjusting the gas flow rate. Examples of such gases include inert gases such as nitrogen, argon, helium, krypton, and xenon, or gases that are inert and stable with respect to the deposition material used for forming the deposited film, and organic EL elements. A mixed gas with an evaporation component such as tris (8-hydroxyquinolinato) aluminum (III) (Alq ₃ ) as a host material or coumarin as a guest material can be used. Further, as the gas 35, an inert gas and a gas containing a component for forming a vapor deposition film are alternately switched and supplied, and a single component vapor deposition film and a multi-component co-vapor deposition film can be alternately formed. .

  As shown in FIG. 8, the second gas introduction portion 31 provided around the vapor deposition source is formed in a region sandwiched between the vapor deposition source 5 and the guide 32 provided around the vapor deposition source. Good. According to this structure, the second gas flow 36 surrounding the gas flow 10 can be formed with a simple configuration.

  As a method of providing the second gas supply portion 33 in the second gas introduction portion 31, in addition to the method of providing one second gas introduction portion 33 shown in FIG. Various modifications shown as a method for introducing the gas 15 into the introduction part 21 can be applied. As shown in FIG. 7 (1), the gas introduction part 31 is provided with gas supply parts at two or more places, or the supply parts 33 are arranged at many places as shown in FIGS. 7 (2) and (3). For example, the shape of the gas supply pipe 34 may be a porous shape having a large number of holes (openings) or a shape having continuous slit-like openings.

  Alternatively, the second gas may be supplied to a buffer space provided below the vapor deposition source, and the second gas may be led out from the buffer space along the peripheral wall of the vapor deposition source. By providing the buffer space, it is possible to form a stable second gas flow with less turbulence.

  9 to 11 are a cross-sectional view (a) and a plan view (b) showing another example of the vapor deposition source and its peripheral device based on the present embodiment.

  Examples 11 to 14 shown in FIGS. 9 to 11 are obtained by adding a means for forming a second gas flow, which is a feature of the present embodiment, to the vapor deposition sources of Examples 2 to 4 of the first embodiment. is there. Accordingly, the devices of Examples 12 to 14 have the characteristics of using the second gas flow described above in combination with the devices of Examples 2 to 4 as well as the devices of Example 11.

  That is, since the apparatus of Example 12 shown in FIG. 9 has the cylindrical portion 20b at the gas outlet 8, the direction of the gas flow 10 can be directed from the vapor deposition source 5 toward the substrate 3, and the vapor deposition material 5a It is possible to increase the utilization efficiency and improve the film formation rate, and to suppress contamination in the vacuum chamber 1.

  Further, since the apparatus of Example 13 shown in FIG. 10 has the buffer space 16, it is possible to supply a stable flow of the gas 15 with less disturbance. Further, since the apparatus of Example 14 shown in FIG. 11 includes the cylindrical portion 20b and the buffer space 16, it has both characteristics.

Embodiment 4
12 to 14 are a cross-sectional view (a) and a plan view (b) showing another example of the vapor deposition source and its peripheral devices based on the present embodiment.

  In Examples 15 to 20 shown in FIGS. 12 to 14, instead of the evaporation source of Example 1 and its peripheral devices used in Embodiment 3, the evaporation sources of Examples 5 to 10 described in Embodiment 2 and the A peripheral device is used, and means for forming a second gas flow is added thereto. These apparatuses are fixed in a vacuum chamber 1 similar to that shown in FIG. 1 and used for forming a deposited film.

  At this time, as already described in the third embodiment, the second gas flow 36 is formed so as to surround the gas flow 10 on the side surface. The flow 37 of vapor molecules to be detached is regulated so as to go toward the substrate 3. That is, the second gas flow 36 functions as a wall (barrier and guide) by gas that prevents the movement of vapor molecules that are going to travel in directions other than the direction of the substrate 3 by molecular collision and directs them toward the direction of the substrate 3. To do.

  Thus, in this embodiment as well, as in the third embodiment, the movement 9 of vapor molecules of the vapor deposition material is doubly controlled by the gas flow 10 and the second gas flow 36. The deposition film can be formed with a uniform film thickness by keeping a sufficient distance between the substrate 3 and the deposition source 5 while keeping the utilization efficiency and deposition rate of the deposition material high. In addition, it is possible to form a high-purity vapor deposition film by minimizing the deposition and deposition of a vapor deposition substance in the vacuum chamber 1 and minimizing contamination in the vacuum chamber 1. Further, by adjusting the respective gas flow rates, the uniformity of the film thickness distribution and the controllability of the film formation rate can be further improved.

Further, by using the second gas flow 36 in combination, it is possible to form a film under a higher degree of vacuum than in the case of the gas flow 10 alone, and the film quality is improved. For example, in order for the second gas stream 36 to function as a wall, the average in the second gas stream 36 is such that the second gas stream 36 does not pass vapor molecules and can be reflected by molecular collisions. The free process may be several cm or less. Since the degree of vacuum corresponding to this is about 10 ⁻¹ Pa, the film can be formed under a higher degree of vacuum than the LPOVPD method.

  Furthermore, the apparatus of Examples 15-20 has the characteristics by using the vapor deposition source of Examples 5-10, and its peripheral device.

  That is, the apparatus of Example 15 has an advantage that the efficiency of taking in vapor molecules released from the surface of the vapor deposition material 5a is higher than that of the apparatus of Example 1. Further, the height in the vertical direction can be reduced, and the whole can be made compact. In addition, the diameter of the opening of the gas outlet 8B can be reduced to the limit necessary to ensure the gas flow rate, the gas flow 10 having a high flow rate can be formed in the vacuum chamber 1, and the vapor molecules can be formed in the substrate 3 Can increase the efficiency of entrainment.

  In the apparatus of Example 16, in addition to the characteristics of the apparatus of Example 15, the cylindrical portion 19 is provided below the outlet 8B, so the direction of the gas flow 10 is directed from the vapor deposition source 25 toward the substrate 3. Therefore, the utilization efficiency of the vapor deposition material 5a can be increased, and contamination in the vacuum chamber 1 can be suppressed. The direction of the cylindrical portion 19 may be provided in the upper direction or both the upper and lower directions (the same applies to Examples 17 to 20). In addition, there is an effect of suppressing the flow of the gas that flows out without flowing near the surface of the vapor deposition material 5a, and improving the uniformity of the concentration of vapor molecules contained in the flowing gas.

  In the apparatus of Example 17, in addition to the characteristics of the apparatus of Example 16, gas flows through the gap sandwiched between the cylindrical portion 19 and the bottom raised portion 26 of the vapor deposition container 25b, so the apparatus gas flow rate of Example 16 is the vapor deposition rate. There is an advantage that it is not affected by the amount of the substance 5a.

  In the apparatus of Example 18, in addition to the characteristics of the apparatus of Example 17, the gas flow rate 12 does not change the flow rate of vapor molecules of the vapor deposition material 5a by the gas flow path 12 penetrating the center of the vapor deposition source 25 from the lower part to the upper part. Can be increased, a strong gas flow 10 can be formed in the vacuum chamber 1, the utilization efficiency of the vapor deposition material 5a can be improved, and contamination in the vacuum chamber 1 can be suppressed.

  In the apparatus of Example 19, in addition to the characteristics of the apparatus of Example 18, the gas 15B flowing through the flow path 12 is supplied from a gas supply pipe 14 different from the gas 15 flowing through the flow path 22 and flows through the flow path 12. The flow rate of 15B can be adjusted independently of the flow rate of the gas 15 flowing through the flow path 22, and the flow rate and concentration of vapor molecules contained in the gas flowing out from the gas outlet 8B can be controlled to a desired value. it can. Further, the gas 15B flowing through the flow path 12 and the gas 15 flowing through the flow path 22 can be different types of gases. For example, one gas is used as a gas containing the constituent components of the vapor deposition film, and multi-component co-deposition is performed. A film can also be formed.

  In the apparatus of Example 20, in addition to the characteristics of the apparatus of Example 18, since the buffer space 27 of the gas 15 is provided below the vapor deposition source 25, a stable flow of the gas 15 with less disturbance is supplied to the vapor deposition source 25. can do.

Embodiment 5
FIG. 15 is a cross-sectional view (a) and a plan view (b) showing a vapor deposition source and its peripheral device of Example 21 based on the present embodiment.

  The apparatus of Example 21 is obtained by removing the upper lid 18 from the apparatus of Example 8 used in the second embodiment. This apparatus is also fixed in a vacuum chamber 1 similar to that shown in FIG.

  At this time, since the upper lid 18 is removed, the gas 15 introduced into the gas introduction part 21 penetrates the central part of the vapor deposition source 25 from the lower part to the upper part according to the pressure difference in the vacuum chamber 1. A gas flow 38 in the central part in the direction toward the direction and a gas flow 39 in the peripheral part from the gas introduction part 21 in the direction toward the substrate 3 are formed. The gas flow 38 in the central portion is surrounded by the wall surface surrounding the gas flow path 12, and the gas flow 39 in the peripheral portion is the two wall surfaces sandwiching the gas introduction portion 21, and the outer peripheral wall protruding portion 20 of the vapor deposition source 5. Orientation is directed toward the substrate 3 by the wall surface and the inner wall surface of the outer wall 17.

  In the vapor deposition source 25, both the inner and outer peripheral walls of the container 25 b are formed so as to protrude, and these peripheral wall protruding portions 20 reflect the vapor molecules of the vapor deposition material 5 a to fly in directions other than the substrate 3. Thus, it functions as a barrier or guide (hot wall) directed toward the substrate 3.

  In a spatial region without the peripheral wall protruding portion 20, the vapor molecule flow 37 that spreads in the left-right direction and tries to deviate from the direction toward the substrate 3 is entrained in the direction of the substrate 3 by the gas flow 38 or 39, or The flight direction of the molecules is regulated so as to be directed toward the substrate 3.

  As described above, the movement 9 of the vapor molecules of the vapor deposition material is controlled by the gas flows 38 and 39. Therefore, by adjusting the gas flow rate, the uniformity of the film thickness distribution and the controllability of the film forming speed are improved. Can be made. At this time, even if the vapor molecules are entrained or the flight direction of the vapor molecules is restricted to be directed toward the substrate 3, the vapor molecules move straight from the vapor deposition source 25 to the substrate 3 in the vacuum chamber 1. Since it is sufficient to support the exercise, the film can be formed under a higher degree of vacuum than the LPOVPD method, and the film quality is improved.

  According to the present embodiment, by using the gas flows 38 and 39 and the peripheral wall protruding portion 20 together, the flight direction of the vapor molecules is guided toward the substrate 3, so that the use efficiency of the deposition material and the film formation speed are increased. While keeping the distance between the substrate 3 and the vapor deposition source 5 sufficiently, the vapor deposition film can be formed with a uniform film thickness. In addition, it is possible to form a high-purity vapor deposition film by minimizing the deposition and deposition of a vapor deposition substance in the vacuum chamber 1 and minimizing contamination in the vacuum chamber 1.

  Further, in the present embodiment, by using the gas flows 38 and 39 in combination, it is not necessary to provide a hot wall in the vicinity of the substrate 3, and there is no fear that the deposited film is heated by the radiant heat from the hot wall. Therefore, the vapor deposition film can be easily maintained at a temperature lower than the melting point of the vapor deposition material to prevent crystallization, and an amorphous organic compound film having smooth surface properties can be formed.

  If the gas flows 38 and 39 are used only for entraining vapor molecules or regulating their flight direction, an inert gas is supplied as gas 15. Examples of the inert gas include nitrogen, argon, helium, krypton, and xenon. However, the inert gas is not limited thereto, and is inert and stable with respect to the vapor deposition material 5a used for forming the vapor deposition film. Any substance can be used. Note that the temperatures of the gas flows 38 and 39 are kept high enough that vapor molecules of the vapor deposition material do not condense in the gas phase.

In addition, if the gas 15 contains the constituent components of the vapor deposition film, a multi-component co-deposition film composed of the vapor deposition material 5a and the constituent components from the gas can be easily formed. At this time, the component ratio can be precisely controlled by adjusting the gas flow rate. Examples of such gases include inert gases such as nitrogen, argon, helium, krypton, and xenon, or gases that are inert and stable with respect to the deposition material used for forming the deposited film, and organic EL elements. A mixed gas with an evaporation component such as tris (8-hydroxyquinolinato) aluminum (III) (Alq ₃ ) as a host material or coumarin as a guest material can be used.

  Further, as the gas 15, an inert gas and a gas containing a component for forming a vapor deposition film are alternately switched and supplied, and a single component vapor deposition film and a multi-component co-vapor deposition film can be alternately formed. .

  FIGS. 15 (2) and 16 are a cross-sectional view (a) and a plan view (b) showing another example of the vapor deposition source and its peripheral devices based on the present embodiment.

  The apparatus of Example 22 shown in FIG. 15 (2) is similar to the apparatus of Example 9 in that the gas 15B flowing through the central flow path 12 is different from the gas 15 introduced into the gas introduction section 21. 14 is configured to be supplied from 14. According to this structure, the flow rate of the gas flow 38 in the central part and the flow rate of the gas flow 39 in the peripheral part can be adjusted independently, and the uniformity of the film thickness distribution and the controllability of the film formation rate can be achieved. Can be improved.

  Further, the gas 15 and the gas 15B can be different types of gases. For example, one gas can be used as a gas containing the constituent components of the vapor deposition film to form a multi-component co-deposition film. At this time, the component ratio of the multi-component co-deposited film can be precisely controlled by adjusting the gas flow rates of the gas 15 and the gas 15B.

  The apparatus of Example 23 shown in FIG. 16 is provided with a buffer space 27 of the gas 15 below the vapor deposition source 25 of the apparatus of Example 21, and the gas 15 is temporarily stored in the buffer space 27, and the vapor deposition source 25 is supplied from the buffer space 27. This is an example in which the gas 15 is supplied. By providing the buffer space 27, it is possible to supply a stable flow of the gas 15 with less disturbance.

Embodiment 6
FIG. 17 is an explanatory diagram showing the configuration of the vapor deposition apparatus based on Embodiment 6 of the present invention. The apparatus shown in FIG. 17 differs from the vapor deposition apparatus of the first embodiment shown in FIG. 1 only in that it has two vapor deposition sources 45a and 45b and gas introduction parts 51a and 51b.

The vacuum chamber 41 is formed of an airtight hollow container provided with an exhaust system 42, and is configured to be evacuated to a high vacuum state of about 1 × 10 ⁻⁵ Pa or more. As a material of the substrate 43 which is a substrate on which the deposited film is formed, any material such as glass, ceramics, metal, or resin can be used depending on the application.

  The substrate support 44 is disposed at the upper center position of the vacuum chamber 41, has a lower surface formed in a planar shape, and is configured to hold the substrate 43 on this surface. The substrate support 44 is provided with a substrate heating heater and a cooling device for heating and / or cooling the substrate 43 to a predetermined temperature, and the chamber 41 measures the temperature of the substrate 43 and the substrate support 44. Temperature measuring means, a controller and power supply for adjusting the power supplied to the heater for heating the substrate in response to a signal from the temperature measuring means, and / or a controller and power supply for adjusting the temperature and flow rate of the cooling refrigerant, and the substrate A fixing means for fixing the support 44 to the chamber 41 is provided.

  Opposite to the substrate 43, two vapor deposition sources 45a and 45b are placed at the lower center position of the vacuum chamber 41. The two vapor deposition sources 45a and 45b are respectively composed of respective vapor deposition materials to be co-deposited and containers for containing them, and below the vapor deposition sources 45a and 45b are evaporation sources for controlling the temperatures of the respective vapor deposition materials. Heating means 46a and 46b are provided. The vapor deposition source heating means 46a and 46b are, for example, a resistance heating type evaporation source heating heater or heating lamp, a temperature measurement means for measuring the temperature of each vapor deposition material, and evaporation according to a signal from the temperature measurement means. It consists of a controller for adjusting the power supplied to the source heating heater and the like, a power source, and the like. In addition, shutters 47a and 47b for controlling the vapor deposition operation are provided above the vapor deposition sources 45a and 45b, respectively.

The vapor deposition material to be co-deposited is not particularly limited. For example, when an organic EL element is formed, Alq ₃ or the like can be used as a host material, and coumarin or the like can be used as a guest material.

  The vapor deposition sources 45a and 45b are respectively provided with gas 55 introduction portions 51a and 51b. The gas introduction part 51a is formed so that the gas flow path penetrates the central part of the vapor deposition source 45a from the lower part to the upper part. The gas introduction part 51b is formed so that the gas flow path penetrates the central part of the vapor deposition source 45b from the lower part to the upper part.

  The operation of depositing vapor molecules of the vapor deposition material on the substrate 43 using the respective vapor deposition sources 45a and 45b is the same as that described in the first embodiment. The vapor deposition sources 45a and 45b are independently controlled, and a common vapor deposition film is formed on the common substrate 3 by performing vapor deposition simultaneously.

  The arrows shown in FIG. 17 indicate the movement directions 49a and 49b of the vapor molecules of the vapor deposition material, and the gas flows 50a and 50b that regulate the movement, respectively. Actually, vapor molecules and gas flow toward the substrate 43 while spreading in the horizontal direction in the figure, so that the vapor deposition materials from the two vapor deposition sources have a constant component ratio on the substrate 43 and a uniform film thickness. The deposited film can be formed.

  The size of the vapor deposition source and the substrate is not particularly limited. For example, the vapor deposition source is a cylinder having a diameter of about 20 mm and a height of about 20 mm, and the substrate has a size of 100 mm × 300 mm. It is about a rectangle. When two or more vapor deposition sources are provided, there is an advantage that more components can be co-deposited than when one vapor deposition source is provided. For example, if two vapor deposition sources and a gas containing a component for forming a vapor deposition film are used in combination, a co-deposition film composed of three components can be formed with good control. At this time, if the vapor deposition sources are too close to each other, there is a possibility that interference by the radiant heat may occur. Can be solved.

Next, a step of forming a co-deposition film using, for example, tris (8-hydroxyquinolinato) aluminum (III) (Alq ₃ ) as a host material and, for example, coumarin as a guest material, using the vapor deposition apparatus shown in FIG. Will be described in more detail. This deposited film is used for an organic EL element, Alq ₃ functions as an electron transport material and a light emitting material, and coumarin functions as a light emitting material.

First, a glass or plastic substrate 43 is fixed to a substrate support 44, Alq ₃ is disposed in a vapor deposition source 45a, and coumarin is disposed in a vapor deposition source 45b, and then the vacuum chamber 1 is subjected to a high vacuum of 1 × 10 ⁻⁵ Pa or higher. Exhaust to the state. At this time, the shutters 47a and 47b are closed.

Next, each temperature adjusting means such as a substrate heating heater of the substrate support 44 and vapor deposition source heating heaters of the vapor deposition source heating means 46a and 46b is energized, and the substrate 43, vapor deposition sources 45a and 45b, and peripheral wall protruding portions Each of 56a and 56b is adjusted to a predetermined temperature. Here, the evaporation source 45a containing a host material such as Alq ₃ can be adjusted to a temperature in the range of 220 to 400 ° C., and the evaporation source 45b containing a guest material such as coumarin can be adjusted to a temperature in the range of 100 to 250 ° C. .

Next, when the temperature of the substrate 43, the vapor deposition sources 45a and 45b, and the peripheral wall protruding portions 56a and 56b reach a predetermined temperature, the shutters 47a and 47b are opened, and Alq ₃ and coumarin vapor molecules are deposited on the substrate 43. Let At this time, the temperature of the vapor deposition source 45a containing Alq ₃ is preferably about 300 ° C., and the temperature of the vapor deposition source 45b containing coumarin is preferably about 150 ° C., for example.

The gas 55 is supplied to the vapor deposition sources 45a and 45b at the start of the above vapor deposition. At this time, the gas temperature is room temperature to 600 ° C., the gas flow rate is 0.1 to 10000 cc / min, and the pressure in the vacuum chamber 41 is 1 × 10 ⁻⁵ to 1 × 10 ³ Pa.

During the formation of the vapor deposition film, for example, the vapor deposition rate of Alq ₃ and coumarin is controlled by the gas flow rate and gas temperature, and the organic co-deposition film containing Alq _{3 as the} host material and coumarin as the guest material is contained in a desired ratio. Is deposited. At this time, since the deposition rate of Alq _{3 as the} host material and coumarin as the guest material is controlled by the gas flow rate and gas temperature, precise control of the component ratio becomes possible, and the responsiveness of the deposition rate control becomes faster. Therefore, it becomes easy to form composition modulation in the film thickness direction.

  In the conventional film formation by the vacuum vapor deposition method, the means for controlling the film formation rate is only the temperature of the vapor deposition source. In the film formation by the vacuum vapor deposition method in which hot wall is introduced, the means for controlling the film formation rate is as follows: Only the temperature of the vapor deposition source and the temperature of the hot wall (however, it is considered that the hot wall is usually set at a constant temperature). Compared with a method having only control means based on these temperatures, according to the present embodiment, in addition to the temperature of the vapor deposition source and the temperature of the peripheral wall protrusions 56a and 56b, control by the gas flow rate and temperature is possible. The deposition rate can be controlled precisely and at high speed, and the controllability is improved. This is particularly effective in the production of the multicomponent co-deposited film described above.

  As mentioned above, although this invention was demonstrated based on embodiment, it cannot be overemphasized that this invention is not limited to these examples at all, and can be suitably changed in the range which does not deviate from the main point of invention.

  The present invention is suitably used for the production of vapor-deposited films, particularly low molecular weight organic compound films used for organic electroluminescence elements, organic semiconductor elements and the like.

Explanatory drawing (a) which shows the structure of the vapor deposition apparatus based on Embodiment 1 of this invention, and the top view of the vapor deposition source seen from the position of the 1b-1b line | wire shown to Fig.1 (a), and its peripheral device ( b). It is sectional drawing (a) and a top view (b) which show the other example of a vapor deposition source and its peripheral device equally. It is sectional drawing (a) and a top view (b) which show the other example of a vapor deposition source and its peripheral device equally. It is sectional drawing (a) and a top view (b) which show the example of a vapor deposition source and its peripheral device based on Embodiment 2 of this invention. It is sectional drawing (a) and a top view (b) which show the other example of a vapor deposition source and its peripheral device equally. It is sectional drawing (a) and a top view (b) which show the other example of a vapor deposition source and its peripheral device equally. It is sectional drawing (a) and a top view (b) which show the other shape of a gas supply part equally. It is sectional drawing (a) and a top view (b) which show the example of a vapor deposition source and its peripheral device based on Embodiment 3 of this invention. It is sectional drawing (a) and a top view (b) which show the other example of a vapor deposition source and its peripheral device equally. It is sectional drawing (a) and a top view (b) which show the other example of a vapor deposition source and its peripheral device equally. It is sectional drawing (a) and a top view (b) which show the other example of a vapor deposition source and its peripheral device equally. It is sectional drawing (a) and the top view (b) which show the example of a vapor deposition source and its peripheral device based on Embodiment 4 of this invention. It is sectional drawing (a) and a top view (b) which show the other example of a vapor deposition source and its peripheral device equally. It is sectional drawing (a) and a top view (b) which show the other example of a vapor deposition source and its peripheral device equally. It is sectional drawing (a) and a top view (b) which show the example of a vapor deposition source and its peripheral device based on Embodiment 5 of this invention. It is sectional drawing (a) and a top view (b) which show the other example of a vapor deposition source and its peripheral device equally. It is explanatory drawing which shows the structure of the vapor deposition apparatus based on Embodiment 6 of this invention. It is explanatory drawing which shows an example of the vacuum evaporation system to which the hot wall method is applied. It is explanatory drawing which shows an example of the vapor deposition apparatus which applied the LPOVPD method.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 ... Vacuum chamber, 2 ... Exhaust system, 3 ... Substrate, 4 ... Substrate support body, 5 ... Deposition source,
5a ... deposition material, 5b ... container containing the deposition material, 6 ... evaporation source heating means, 7 ... shutter,
8, 8B ... Gas outlet, 9 ... Direction of vapor molecule movement of vapor deposition material, 10 ... Gas flow,
DESCRIPTION OF SYMBOLS 11 ... Gas introduction part, 12 ... Gas flow path, 13 ... Gas supply part, 14 ... Gas supply pipe | tube,
15, 15B ... gas, 16 ... buffer space, 17 ... outer wall, 18 ... top cover,
DESCRIPTION OF SYMBOLS 19 ... Cylindrical part, 20 ... Peripheral wall protrusion part, 20a ... Peripheral wall diameter reduction part, 20b ... Cylindrical part,
20c ... projecting end, 21 ... gas introduction part, 22 ... gas flow path, 23 ... gas supply part,
24 ... Gas supply pipe, 25 ... Vapor deposition source, 25b ... Container for containing vapor deposition material, 26 ... Raised portion,
27 ... Buffer space, 28 ... Hole (opening), 29 ... Slit-like opening,
31 ... Second gas introduction unit, 32 ... Guide, 33 ... Second gas supply unit,
34 ... Second gas supply tank 35 ... Second gas 36 ... Second gas flow,
37 ... the flow of vapor molecules trying to spread in the left-right direction, 38 ... the flow of gas in the center,
39 ... Peripheral gas flow, 41 ... Vacuum chamber, 42 ... Exhaust system, 43 ... Substrate,
44 ... Substrate support, 45a, 45b ... Deposition source, 46a, 46b ... Evaporation source heating means,
47a, 47b ... shutter, 48a, 48b ... gas outlet,
49a, 49b ... direction of movement of vapor molecules, 50a, 50b ... gas flow,
51a, 51b ... gas introduction part, 55 ... gas, 56a, 56b ... peripheral wall protrusion part,
61 ... Vacuum chamber, 62 ... Exhaust device, 63 ... Deposition source, 64 ... Substrate,
65 ... inner wall (hot wall), 66 ... heater for heating the inner wall, 70 ... reactor,
71 ... carrier gas supply system, 72 ... crucible, 73 ... bubbler, 74 ... reactive gas inlet,
75 ... Reactor, 76 ... Multi-region heater / cooler, 77 ... Substrate, 78 ... Substrate temperature control block

Claims (34)

  When forming the vapor deposition film on the substrate, the substrate and the vapor deposition source are opposed to each other, and a gas flow is formed from a region inside the circumference of the vapor deposition source toward the substrate, and the vapor flow causes the vapor deposition. A vapor deposition method for entraining a vapor deposition material released from a source toward the substrate.   The vapor deposition method according to claim 1, wherein the gas is allowed to flow through the vapor deposition source.   The vapor deposition method according to claim 1, wherein the gas is flowed from a peripheral portion of the vapor deposition source toward an upper central portion, and the vapor deposition material is entrained by the gas flow.   2. The vapor deposition according to claim 1, wherein the gas is caused to flow through the vapor deposition source, the gas is caused to flow from a peripheral portion of the vapor deposition source toward an upper center portion, and the vapor deposition material is entrained by the gas flow. Method.   The vapor deposition method according to claim 1, wherein a gas outlet port from the vapor deposition source is narrowed.   The vapor deposition method according to claim 5, wherein the outlet is cylindrical.   The vapor deposition method according to claim 6, wherein the cylindrical portion of the outlet port is directed upward and / or downward.   The vapor deposition method according to claim 1, wherein an outer wall surrounding an outer periphery of the vapor deposition source is provided, and the gas is introduced between the outer wall and the vapor deposition source.   The vapor deposition method according to claim 1, wherein a buffer space for the gas is provided below the vapor deposition source.   The vapor deposition method according to claim 1, wherein an inert gas is used as the gas.   The vapor deposition method according to claim 1, wherein a gas containing a component that forms the vapor deposition film is used as the gas.   The inert gas and the gas containing the component which forms the said vapor deposition film are supplied by switching alternately as said gas, and a single component vapor deposition film and a co-vapor deposition film are formed into a film alternately. Vapor deposition method.   The vapor deposition method according to claim 11 or 12, wherein the component forming the vapor deposition film is an organic compound.   The vapor deposition source and the container containing the vapor deposition material constitute the vapor deposition source, the peripheral wall of the container projects toward the base, and a predetermined gap is formed between the protruding end of the peripheral wall and the base. The vapor deposition method according to claim 1, wherein a distance is provided.   The vapor deposition method of Claim 14 which heats the surrounding wall of the said container.   The vapor deposition method according to claim 1, wherein a thin film of an organic compound is formed as the vapor deposition film.   In addition to the gas flow, a second gas flow is formed from the periphery of the vapor deposition source toward the substrate, and the flight direction of the vapor deposition material released from the vapor deposition source by the second gas flow is determined. The vapor deposition method according to claim 1, wherein the vapor deposition method is regulated in a direction of the substrate.   The vapor deposition method according to claim 17, wherein a buffer space for the second gas is provided below the vapor deposition source.   19. A vapor deposition apparatus used for carrying out the vapor deposition method according to claim 1, wherein the substrate and the vapor deposition source are provided in a vacuum chamber, and are located inside a periphery of the vapor deposition source. A vapor deposition apparatus comprising means for forming a gas flow from the region of the gas flow toward the substrate.   The vapor deposition apparatus according to claim 19, wherein the gas flow path is formed so as to penetrate a central portion of the vapor deposition source from the lower part to the upper part.   The vapor deposition apparatus according to claim 19, wherein the gas flow path is formed from a peripheral portion of the vapor deposition source toward an upper central portion thereof.   The gas flow path is formed so as to penetrate the central part of the vapor deposition source from the lower part to the upper part, and is formed from the peripheral part of the vapor deposition source toward the upper central part thereof. Deposition apparatus described.   The vapor deposition apparatus of Claim 19 with which the outlet port of the said gas from the said vapor deposition source is narrowed.   The vapor deposition apparatus according to claim 23, wherein the outlet port is formed in a cylindrical shape.   The vapor deposition apparatus according to claim 24, wherein the cylindrical portion of the outlet port is directed upward and / or downward.   The vapor deposition apparatus according to claim 19, wherein an outer wall surrounding an outer periphery of the vapor deposition source is provided, and the gas is introduced between the outer wall and the vapor deposition source.   The vapor deposition apparatus according to claim 19, wherein the gas buffer space is provided below the vapor deposition source.   The vapor deposition source is constituted by a vapor deposition material and a container for containing the vapor deposition material, and a peripheral wall of the container protrudes toward the base, and a predetermined gap is provided between the protruding end of the peripheral wall and the base. The vapor deposition apparatus according to claim 19, wherein a distance of   The vapor deposition apparatus according to claim 28, wherein a peripheral wall of the container is heated.   30. The method according to claim 19, further comprising a second gas introduction portion around the vapor deposition source in addition to means for forming a gas flow from a region inside the circumference of the vapor deposition source toward the substrate. The vapor deposition apparatus described in any one of the items.   31. The vapor deposition apparatus according to claim 30, wherein the second gas introduction part is formed in a region sandwiched between the vapor deposition source and a guide provided around the vapor deposition source.   The vapor deposition according to claim 30, wherein the second gas is supplied to a buffer space provided at a lower portion of the vapor deposition source, and the second gas is led out from the buffer space along a peripheral wall of the vapor deposition source. apparatus.   The vapor deposition apparatus according to claim 19 or 30, wherein the gas supply section is provided at one or a plurality of positions with respect to the gas introduction section. 34. The vapor deposition apparatus according to claim 33, wherein the gas supply unit opens in a porous or slit shape with respect to the gas introduction unit along a peripheral wall of the vapor deposition source.

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