JP2014070238A - Vacuum evaporation device, and evaporation method for the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a vacuum deposition device capable of shortening one of a total maintenance time period or a precoating time period so as to shorten a total maintenance time period, and mounting a material which has been difficult to deposit on a crystal oscillator, and provide an evaporation method for the vacuum evaporation device.SOLUTION: A vacuum deposition device comprises: at least two evaporation sources arranged in a vacuum chamber; and film thickness sensors disposed to correspond individually to the evaporation sources. In the film thickness sensor of an adhesion-reluctant material owned by one of the evaporation sources, there is introduced a material owned by the other evaporation source.

Description

  The present invention relates to a vacuum deposition apparatus and a deposition method thereof.

  During the organic EL device manufacturing process, the crystal resonator is controlled in a film thickness in a vacuum state. This crystal resonator has a circular shape, and a metal film (underlayer such as nickel or chromium + film such as gold) having a size approximately half of the outer diameter is formed.

  The principle uses the fact that the oscillation frequency changes depending on the weight of the film attached to the crystal resonator. By detecting the decrease in the oscillation frequency, the film thickness is calculated from the film weight and controlled. Therefore, the rate value (hereinafter referred to as the rate value) of the crystal resonator plays an extremely important role in controlling the film thickness.

  Thus, the film thickness control utilizes the principle that the frequency is reduced by the material adhering to the crystal resonator. However, there are materials that are difficult to adhere to the surface of the crystal unit, and there are cases where an accurate evaporation rate value cannot be detected. Magnesium is taken up as a material that is difficult to adhere.

  For materials that are difficult to adhere, the actual evaporation rate and the detection rate are completely different until the pre-coat (hereinafter referred to as precoat) is completed, and the detection rate value is several times lower.

  As a prior art, there is a pre-coating operation in which magnesium is deposited on a quartz resonator in order to accurately detect the evaporation rate when depositing magnesium. In order to shorten the time for this pre-coating operation, the pre-coating operation is performed by producing 7 to 10 times the vapor necessary for the normal device process. Even under such circumstances, one crystal oscillator requires 3 to 4 hours of pre-coating time. As another shortening measure, we examined a method of pre-coating in parallel during production.

  This system is a system in which a shutter is provided in the mechanism of the crystal unit, the shutter is opened during production, and the crystal unit to be used next is precoated.

  The problem here is that the former method requires a lot of time until the start of production, and because it generates 7 to 10 times more steam, it requires a lot of pre-coating material and the amount of material consumption increases. is there.

  In the latter method, the pre-coating time performed during production is shortened, but the pre-coating time of the crystal unit used for production after the apparatus is started up is required. Also, like the former, a precoat material is also required, which affects the material consumption.

JP-A-5-320901 JP-A-5-320902 JP-A-7-118847 JP 2005-325400 A

  In recent years, development of metal evaporation sources for large substrates has been progressing. Among them, a crystal resonator is used for film thickness control, and the crystal resonator is a multiple type in order to extend the operation time. In order to pre-coat all the quartz crystal resonators, 7 to 10 times as much steam as necessary in the device process is emitted as described above. In addition, since a single crystal resonator takes 3 to 4 hours of pre-coating time, enormous time and materials are required.

  In an organic EL manufacturing apparatus, there is currently no means for controlling the film thickness in a vacuum except relying on the detection rate value (Rate value) of the crystal resonator. Therefore, the accuracy of the detection rate value of the crystal resonator is an important key point. In order to improve the reliability of the rate value, it is important to adhere the evaporated material without flipping it on the surface of the crystal unit.

  Materials that are difficult to adhere to a crystal unit such as magnesium are pre-coated before production, and are accelerated in abundant vapor by applying high power to accelerate the time. It must be kept in mind that material consumption will increase by applying high power.

At the same time, regular maintenance is performed to fill the material in the organic EL manufacturing process. When the material is consumed, the heater is dropped and the chamber is opened. After a series of maintenance such as replacement of the crucible filled with the material, replacement of the crystal resonator, replacement of the mask, etc., the temperature is raised again.
How to shorten the production stop time is an important issue item, and the same is true for the shortening of the pre-coating time described above.

  In addition, in the method of pre-coating the next crystal unit to be used in parallel during production, the pre-coated crystal unit is defective (NG product) or pre-coating has been completed during production. If not, there is a problem that production must be interrupted until completion. In addition, as described above, when measuring the deposition rate of a material (magnesium) that does not easily adhere to the surface of the crystal unit, there is a problem that an accurate evaporation rate value cannot be detected.

  In order to solve the above-described problems, the present invention can reduce the total maintenance time, shorten the pre-coating time, which is one of them, and allow the material that has been difficult to adhere to the crystal unit to be attached. The object is to provide a vacuum deposition apparatus and a deposition method therefor.

  In order to solve the above-mentioned problems, the present invention has at least two or more evaporation sources disposed in a vacuum chamber, and a film thickness sensor installed corresponding to each of the evaporation sources, Among these, the material possessed by the other evaporation source is introduced into the film thickness sensor of the material that is difficult to adhere to the one evaporation source.

  According to the present invention, a vacuum deposition apparatus capable of further reducing the pre-coating time, which is one of them, and making it possible to attach a material that has been difficult to adhere to a crystal resonator, and its A vapor deposition method can be provided.

It is a disassembled perspective view of the evaporation source apparatus which concerns on the Example of this invention. It is sectional drawing of the thin film forming apparatus provided with the evaporation source apparatus which concerns on the Example of this invention. It is a perspective view of the evaporation source device concerning Example 1 of the present invention. It is a front view of the crystal resonator based on Example 1 of this invention. It is a perspective view of the film thickness control apparatus for silver which concerns on Example 1 of this invention. It is a perspective view of the film thickness control apparatus for magnesium which concerns on Example 1 of this invention. It is sectional drawing of the evaporation source which concerns on Example 2 of this invention. It is a perspective view of the film thickness control apparatus for silver which concerns on Example 2 of this invention. It is a side view of the film thickness control apparatus for silver which concerns on Example 2 of this invention. It is a flowchart explaining the vapor deposition method by this invention.

  Hereinafter, embodiments of the organic EL device manufacturing apparatus of the present invention will be described with reference to FIGS.

  In the organic EL device apparatus according to the present embodiment, the substrate to be processed, which is carried in from the load lock chamber 1 that is processed from the atmosphere to a vacuum state, is transferred to the vapor deposition chamber through a certain process. Further, in this embodiment, the substrate is transported with the vapor deposition surface as the upper surface, and vapor deposition is performed with the substrate vertical.

  The organic EL device device has a multilayer structure in which various materials such as a hole injection layer, a transport layer, an electron injection layer, a transport layer, and a metal material are stacked in a thin film in addition to a light emitting material layer.

  FIG. 1 is an exploded perspective view of an evaporation source apparatus according to an embodiment of the present invention.

  In FIG. 1, an EL material evaporation source device 1 includes a casing 2 (water-cooled shield box) elongated in one horizontal direction, and a magnesium crucible 3 and a silver crucible 4 are indicated by arrows inside the casing 2. Pay from the direction. The silver crucible 4 is located below the magnesium crucible 2 and is divided into four pieces. A heating device 5 (heater) for heating both the crucibles 3 and 4 at a predetermined temperature is attached around each crucible 3 and 4 as shown in FIG.

  Gas discharge plates 3a and 4a are attached to the front surfaces of the crucibles 3 and 4, respectively. A plurality of gas discharge holes 3b and 4b are uniformly formed in the gas discharge plates 3a and 4a in the horizontal direction. The gas discharge holes 3b and 4b are formed so that the distance between both ends is closer than the distance at the center.

  FIG. 2 is a cross-sectional view of a thin film forming apparatus provided with an evaporation source apparatus according to an embodiment of the present invention.

  In FIG. 2, the evaporation source device 1 is accommodated in a vacuum chamber 7 indicated by a dotted line. In the vacuum chamber 7, a deposition target substrate 8 such as a glass plate for manufacturing an organic EL device is fixed upright by a holding device (not shown). The evaporation source apparatus 1 moves up and down with respect to the deposition target substrate 8 as indicated by an arrow. The evaporation source device 1 injects the vaporized particles 3c and 4c of the organic EL device material 6 which are gasified by heating by the heating device 5 from the gas discharge holes 3b and 4b while moving up and down. It is like that. As a result, the evaporated particles 3 c and 4 c of the organic EL device material 6 are widely deposited on the surface of the deposition target substrate 8.

  FIG. 3 is a perspective view of the evaporation source apparatus according to Embodiment 1 of the present invention.

  FIG. 3 is a perspective view of an evaporation source apparatus provided with an embodiment of the present invention. FIG. 3 is drawn with the gas release plate removed for convenience of explanation.

  In FIG. 3, as mentioned above, the crucible 3 for magnesium is attached to the upper stage in the housing | casing 2 provided with the cooling mechanism (not shown). At both ends of the magnesium crucible 3, a magnesium film thickness control device 9 (also referred to as a film thickness sensor) having a crystal resonator for controlling the film thickness is installed. The magnesium film thickness control device 9 is connected to a crystal resonator, and includes an introduction tube 10 (also referred to as a nozzle) facing the magnesium crucible 3 and a silver precoat introduction tube 11 facing the silver crucible 4. .

  On the other hand, in the lower stage, a silver crucible 4 is attached in a housing 2 provided with a cooling mechanism (not shown) in the same manner as the magnesium crucible 3. At both ends of the silver crucible 4, a first silver film thickness control device 12 having a crystal resonator for film thickness control is installed. The first silver film thickness control device 12 is provided with an introduction tube 13 connected to a crystal resonator.

  The introduction pipe 13 of the first silver film thickness control device 12 is directed to the crucibles 4 at both ends as indicated by dotted arrows among the four silver crucibles 4 divided. Below the first silver film thickness control device 12, a second silver film thickness control device 12a is attached. Of the silver crucible 4 divided into four, the introduction pipe 13a of the second silver film thickness controller 12a is directed to the two central crucibles as indicated by the dotted arrows.

  Here, the structure of each crucible 3, 4 will be described. The magnesium crucible 3 has an organic EL device material 6 to be deposited, and a stable deposition rate can be obtained by controlling the heating with the heating device 5. A plurality of gas discharge holes are arranged in front of the crucible 3, and a material evaporated by heating is ejected from the gas discharge holes.

  The lower crucible 4 for silver has a shorter width than the crucible 3 for magnesium, and a plurality of silver crucibles 4 are installed in a horizontal row (in this embodiment, four are used, but the number is not limited to this). Similar to the crucible 3 for magnesium, the silver crucible 4 has an organic EL device material 6 deposited inside, and a plurality of gas discharge holes 4 b are arranged on the front surface of the crucible 4. The silver crucible 4 is individually controlled from the gas discharge hole 4b, heated by each control, and vaporized vapor deposition particles 4c are jetted.

  Since the crucible 4 for silver has a plurality of crucibles arranged in a horizontal row, it is necessary to adjust the film thickness before film formation of the organic EL device. When adjusting the film thickness, silver pre-coating of the first crystal unit is performed. The second and subsequent silver precoats are performed when the organic EL device is formed.

  Next, the configuration of the entire crystal unit for controlling the film thickness used in this embodiment will be described with reference to FIGS.

  FIG. 4 is a front view of the crystal resonator according to the embodiment of the present invention.

  In FIG. 4, twelve crystal resonators 14 having a diameter of about 20 mm are mounted on a disk-like retainer 15 in a ring shape. Thick film control by the crystal unit 14 is to detect the thickness of the metal film attached to the deposition target substrate 8 by utilizing the fact that the oscillation frequency is lowered when the metal film is attached to the crystal unit 14.

  FIG. 5 is a perspective view of a film thickness control apparatus for silver according to an embodiment of the present invention.

  In FIG. 5, the first silver film thickness control device 12 includes a retainer 15 having a mechanism for electrically controlling the crystal resonator 14 shown in FIG. The retainer 15 is held by a retainer holder 16. The first silver film thickness control device 12 includes a cooling jacket 17 having an electrical processing mechanism for the crystal resonator 14 therein.

  As described above, the quartz resonator 14 needs to be replaced periodically because the metal film adheres to some extent and the frequency decreases and accurate film thickness control cannot be performed. Therefore, the retainer 15 is provided with a plurality of crystal resonators 14 and is constituted by an introduction tube 18 for introducing silver particles before the crystal resonator 14 to be used.

  The second silver film thickness control device 12a has the same configuration as the first silver film thickness control device 12, and therefore the description thereof is omitted.

  Next, the magnesium film thickness control device will be described.

  FIG. 6 is a perspective view of a magnesium film thickness control apparatus according to an embodiment of the present invention.

  In FIG. 6, the magnesium film thickness control device 9 includes a retainer 19 having a mechanism for electrically controlling the crystal resonator 14 shown in FIG. The retainer 19 is held by a retainer holder 20. Further, the magnesium film thickness control device 9 includes a cooling jacket 21 having an electrical processing mechanism for the crystal resonator 14 therein. The magnesium film thickness control device 9 is also provided with an introduction pipe 10 for introducing magnesium particles, but the difference in configuration from that for silver is that the silver film in the lower stage is used for the film thickness control mechanism for magnesium. A silver precoat introduction pipe 11 for introduction is provided.

  Here, a silver precoat for realizing the present invention will be described.

  As shown in FIG. 3, recently, co-evaporation in which silver and magnesium are simultaneously deposited in one chamber has become common. Therefore, in the embodiment of the present invention, silver is first attached to the magnesium detecting crystal resonator.

  In other words, since magnesium is a material that does not easily adhere to the crystal unit, pre-coating is performed before production (in order to accelerate the time, high power is applied to make the vapor state rich). However, in the present embodiment, silver is previously attached to the crystal unit in response to the problem that the material consumption increases due to application of high power. As a result, magnesium can be attached to the crystal resonator. In other words, silver is a kind of adhesive for magnesium for the crystal unit.

  Next, in this embodiment, silver is first adhered to the quartz crystal for detecting magnesium. Silver precoat control for reducing precoat time and realizing accurate film thickness control will be described below.

  The quartz resonator uses the principle that the film thickness is calculated from the weight of the film by utilizing the fact that the oscillation frequency is lowered depending on the weight of the attached film. Therefore, the frequency reduction of substances having different densities of silver and magnesium is naturally different.

  By attaching silver first, the frequency reduction of magnesium, so-called detection rate value should not be affected. Here, it is a condition that the silver can be detected immediately so that the rate of magnesium can be detected and the rate value of the magnesium crystal resonator can be accurately displayed.

  Here, an embodiment will be described with reference to FIG. 7 in which silver is deposited so that the above rate detection can be performed immediately and the rate value of the crystal unit for magnesium can be accurately measured.

  FIG. 7 is a cross-sectional view of an evaporation source according to Embodiment 2 of the present invention.

  7, in this embodiment, in addition to the structure of the evaporation source 1 shown in FIG. 3, angle limiting plates 22 and 23 for controlling film quality and film thickness are provided. That is, the angle limiting plates 22 and 23 are attached in the gas injection direction of the plurality of gas discharge holes 3b and 4b provided in the gas discharge plates 3a and 4a shown in FIG.

  The angle limiting plates 22 and 23 are attached in front of the material crucibles 3 and 4 (in the gas injection direction), and the magnesium angle limiting plate 22 is attached in front of the magnesium crucible 3. A silver angle limiting plate 23 is attached in front of the silver crucible 4.

  FIG. 8 is a perspective view of the silver film thickness control apparatus according to the second embodiment of the present invention.

  FIG. 9 is a side view of the silver film thickness control apparatus according to the second embodiment of the present invention.

  8 and 9, a silver pre-coating introduction tube 11 of the magnesium film thickness control device 9 is connected to the silver angle limiting plate 23, and a shutter for controlling an appropriate silver adhesion amount is in front of it. 24 is attached.

  Thus, according to the present embodiment, replacement adjustment of the crystal resonator can be easily performed by the shutter.

  By the way, at the time of pre-coating the first sheet after filling the material, at the time of adjusting the film thickness of silver, while the crystal unit used for the second and subsequent sheets is within the usable range, both of them are replaced. The shutter 24 is opened before and the shutter 24 is closed when an appropriate silver film adheres to the crystal unit (the timing of opening the shutter 24 does not matter. However, when the crystal unit needs to be replaced) The silver precoat must be completed).

Here, the optimum silver adhesion amount and silver pre-coating time for the crystal unit for magnesium are defined.
(1) Since a crystal oscillator cannot display an accurate rate when a certain amount of material is adhered, it is replaced with the next crystal oscillator at an appropriate timing.
(2) With respect to the lifetime when the crystal resonator is used effectively at 100 [%], the appropriate timing is the replacement timing when using about 7-12 [%].
(3) When the deposition rate is about 0.3 to 0.4 [３〜 / sec], replace with a new crystal unit at about 30 to 35 [H].
(4) On the other hand, when the optimal silver precoat film thickness is about 100 to 1000 [Å] and the evaporation rate is 0.2 [Å / sec], the shutter has an opening time of 0.14 to 1.4 [H]. And
(5) Therefore, silver pre-coating of about 0.14 to 1.4 [H] is performed during the effective time 30 to 35 [H] of one crystal resonator.
(6) Since this pre-coating possibility judgment is provided with a detection mechanism similar to the detection mechanism performing the film thickness control, it can be judged there.

  FIG. 10 is a flowchart for explaining a vapor deposition method according to the present invention.

  In FIG. 10, it is determined in step 100 whether the vapor deposition material is a material that is difficult to adhere to the crystal resonator, such as magnesium. In the case of NO, normal vapor deposition is performed in step 101. In the case of YES, it is determined in step 102 whether the crystal unit being used can be used continuously. In the case of NO, a new crystal unit is replaced in step 103, and in the case of YES, an adhesive material (silver) is attached to the crystal unit with a nozzle in step 104. In step 105, the adhesion amount of the adhesive material is determined. In the case of NO, the nozzle shutter is closed in step 106, and in the case of OK, in step 107, a material that is difficult to adhere is adhered on the adhesive material.

  According to the flow of FIG. 10 described above, it is possible to provide an organic EL device manufacturing apparatus capable of detecting a precoat such as magnesium that is difficult to adhere to a crystal resonator much earlier, and manufacturing an organic EL device with a high operating rate. Can provide a method.

  In the above description, the organic EL device has been described as an example.

  According to the present embodiment, it is possible to detect the rate of magnesium much faster by attaching silver that is likely to adhere to the quartz vibrator for detecting the magnesium rate first. In general, gold, silver, and aluminum alloy are used for the electrodes of the crystal unit. However, the crystal unit once exposed to the atmosphere is contaminated with organic substances. The organic matter further hinders material adhesion. Therefore, the crystal unit with silver attached can be used in the production process without being exposed to the atmosphere.

  In the unlikely event that the crystal unit is defective (NG product), silver adheres quickly, so in such cases, silver pre-coating can be performed immediately, and production interruption due to pre-coating can be minimized.

  As described above, according to the present invention, it is possible to provide an organic EL device manufacturing apparatus, an organic EL device manufacturing method, a film forming apparatus, or a film forming method that can detect magnesium precoat much more quickly. Further, according to the present invention, it is possible to provide an organic EL device manufacturing apparatus, an organic EL device manufacturing method, a film forming apparatus, or a film forming method with high productivity.

  Furthermore, according to the present invention, it is possible to provide an organic EL device manufacturing apparatus, an organic EL device manufacturing method, a film forming apparatus, or a film forming method with a high operating rate.

  Further, according to the present invention, an organic EL device manufacturing apparatus and an organic EL device film forming apparatus are used for a material (mainly magnesium) whose rate is difficult to detect in a method of forming a film using a crystal resonator. It is possible to provide a vacuum vapor deposition apparatus and a vapor deposition method capable of shortening the precoat time.

1 ... evaporation source device, 2 ... housing,
3 ... crucible for magnesium, 3a ... gas release plate,
3b ... gas release hole, 3c ... deposited particles,
4 ... Silver crucible, 4a ... Gas release plate,
4b ... gas discharge hole, 4c ... vapor deposition particle,
5 ... Heating device, 6 ... Organic EL device material,
7 ... Vacuum chamber, 8 ... Deposition substrate,
9 ... Film thickness control device for magnesium, 10 ... Introduction pipe,
11 ... Introduction pipe for silver precoat, 12 ... First film thickness controller for silver,
12a ... Secondly, a film thickness control device for silver, 13 ... Introducing pipe,
13a ... introducing tube, 14 ... crystal resonator,
15 ... Retainer, 16 ... Retainer holder,
17 ... Cooling jacket, 18 ... Introduction pipe,
19 ... Retainer, 20 ... Retainer holder,
21 ... Cooling jacket, 22 ... Angle limiting plate,
23: Angle limiting plate, 24: Shutter.

Claims (6)

And having at least two or more evaporation sources arranged in the vacuum chamber, and a film thickness sensor installed corresponding to each of the evaporation sources,
The vacuum evaporation apparatus characterized by introducing the material which the other evaporation source has into the said film thickness sensor of the material which is hard to adhere to one evaporation source among the said evaporation sources. The vacuum evaporation apparatus according to claim 1, wherein
2. The vacuum deposition apparatus according to claim 1, wherein the material that hardly adheres is magnesium, and the material of the other evaporation source is silver. In the vacuum evaporation apparatus in any one of Claim 1 or 2,
The vacuum deposition apparatus, wherein the film thickness sensor includes a nozzle for introducing the magnesium and a nozzle for introducing silver. In the vacuum evaporation system in any one of Claims 1 thru | or 3,
A vacuum deposition apparatus, wherein the silver nozzle attached to the film thickness sensor is provided with a shutter for controlling the amount of silver deposited, and a silver angle limiting plate is provided in the vicinity of the shutter. In the vacuum evaporation system in any one of Claims 1 thru | or 4,
The vacuum deposition apparatus, wherein the film thickness sensor includes at least two crystal resonators. Steps to determine whether the material is difficult to adhere to the crystal unit,
Determining whether the quartz crystal in use can be used continuously;
A step of attaching an adhesive material to the crystal unit with a nozzle;
A step to determine whether the application amount of the adhesive material is appropriate;
Step to apply a material that does not easily adhere to the adhesive material of the crystal unit,
A vacuum deposition method comprising:

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