JP2016130336A - Method of manufacturing vapor-deposited film and vapor deposition apparatus - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method of manufacturing a vapor-deposited film in which a vapor deposition rate (film forming speed) can be precisely controlled to a desired target value while the lifetime of a vapor deposition sensor is prolonged.SOLUTION: A method of manufacturing a vapor-deposited film includes: a first control process of performing feedback control to manipulate electric power supplied to heating means 12 so that while a vapor deposition rate is measured with a shutter 31 of a vapor deposition rate sensor 3 open, a deviation of a vapor deposition rate measured value PV1 from a target vapor deposition rate set value SV1 becomes small; and a determination process of determining whether an amount of variation in the vapor deposition rate measured value is within a predetermined range, and closing the shutter and then interrupting the first control process; and a second control process of setting a temperature PV2 of a container as a target temperature sensor value on the determination, and performing feedback control to manipulate the electric power so that a deviation of a temperature measured value PV2 from the target temperature set value becomes small while the temperature of the container is measured by a temperature sensor 4.SELECTED DRAWING: Figure 3

Description

  The present invention relates to a method for manufacturing a vapor deposition film and a vapor deposition apparatus used when forming an organic electroluminescence element or the like. In particular, the present invention is a method for producing a vapor deposition film capable of accurately controlling the vapor deposition rate (deposition rate) to a desired target value while extending the life of the vapor deposition rate sensor for measuring the vapor deposition rate by adhering a vapor deposition material And an evaporation apparatus.

  An organic electroluminescence (hereinafter, “electric luminescence” is appropriately referred to as “EL”) apparatus includes a base material and an organic EL element provided on the base material. In addition to the organic film functioning as the light emitting layer, the organic EL element requires a pair of electrode films sandwiching the organic film in order to supply a driving voltage to the organic film.

As a method for forming an organic film or an electrode film that constitutes an organic EL element, a vacuum deposition method, a coating method, or the like is generally known. Among these, vacuum deposition is widely used because the purity of the material for forming the organic film and the electrode film can be increased and an organic EL element having a long lifetime can be easily formed.
A vapor deposition apparatus for performing a vacuum vapor deposition method generally includes a vacuum chamber and a vapor deposition source that is provided in the vacuum chamber and is disposed to face a base material that forms a vapor deposition film. The vapor deposition source includes a container (such as a crucible) that stores a vapor deposition material and a heating unit that heats the container. By heating the container by the heating means, the vapor deposition material evaporated from the container is released and deposited on the base material, whereby a vapor deposition film is formed on the base material.

As a vapor deposition apparatus, a method of forming a vapor deposition film on a sheet-like substrate (batch method) and a method of forming a vapor deposition film on the substrate while conveying a long belt-shaped substrate between rolls (roll) (Two-roll method) is known (see, for example, Patent Document 1 as a roll-to-roll vapor deposition apparatus).
A roll-to-roll type vapor deposition apparatus is advantageous in that a vapor deposition film can be formed at a high speed (a high vapor deposition rate).

Since the film thickness accuracy of the deposited film is a very important factor that affects the light emission characteristics and life of the organic EL element, the deposition rate that affects the film thickness accuracy is kept constant (accurately controlled to the desired target value). It is important to.
In particular, in the case of a roll-to-roll type vapor deposition apparatus, since the vapor deposition rate is high, in order to prevent mass production of defective products, it is important to stabilize the vapor deposition rate in a short time from the start of vapor deposition and also to stabilize for a long time. It is.

  Conventionally, the deposition rate is controlled in a configuration as shown in the block diagram of FIG. That is, the container 11 containing the vapor deposition material constituting the vapor deposition source 1 is heated by the heating means 12 to start the formation of the vapor deposition film on the substrate S and the vapor deposition rate sensor 3 is used to measure the vapor deposition rate. . The target vapor deposition rate set value SV1 is set and stored in advance in the control means 5A, and the vapor deposition rate measured value PV1 measured using the vapor deposition rate sensor 3 is input. The control unit 5A operates the power supplied to the heating unit 12 so that the deviation between the target deposition rate set value SV1 and the measured deposition rate PV1 is small (the power set value of the power source 2 that supplies power to the heating unit 12). Feedback control (PID control) is performed (operating MV2).

Here, as the deposition rate sensor 3, a QCM (Quartz Crystal Microbalance) sensor to which a deposition material is attached is preferably used.
The QCM sensor is a sensor that measures the attached mass from the amount of decrease in the resonance frequency by utilizing the property that the resonance frequency is reduced according to the mass when a substance is attached to the electrode surface of the crystal resonator. By measuring the mass of the vapor deposition material deposited per unit time with the QCM sensor, it is possible to calculate the deposition amount of the vapor deposition material deposited on the substrate S per unit time, that is, the vapor deposition rate (film formation rate). It is.
When a QCM sensor is used as the deposition rate sensor 3, particularly when a metal material having a large mass, such as an electrode film of an organic EL element, is deposited on the substrate S, the metal material adheres to the QCM sensor, so that the sensor There is a problem that the lifetime is significantly reduced. In order to replace a QCM sensor that has reached the end of its life with a new one, it is necessary to lower the temperature of the container 11 and wait for the temperature in the vacuum chamber to drop before starting the replacement operation. Moreover, in order to resume the vapor deposition, it is necessary to make the degree of vacuum in the vacuum chamber a high vacuum of about 10 ⁻⁵ Pa, so that a dead time of substantially one day occurs.

  According to the conventional method for controlling a deposition rate, it is possible to stabilize the deposition rate in a relatively short time from the start of deposition. However, when a sensor that measures the deposition rate by attaching a deposition material such as a QCM sensor is used as the deposition rate sensor 3, it is difficult to stabilize for a long time due to the lifetime of the deposition rate sensor 3. . In addition, if the lifetime of the vapor deposition rate sensor 3 is exhausted in a short time, it is necessary to frequently perform an exchange operation that requires labor, and thus there is a problem that the production efficiency of the vapor deposition film is lowered.

JP 2012-140695 A

  The present invention has been made in order to solve the above-described problems of the prior art. The deposition rate (film formation) is achieved while extending the lifetime of the deposition rate sensor that measures the deposition rate by attaching a deposition material. It is an object of the present invention to provide a vapor deposition film manufacturing method and a vapor deposition apparatus capable of accurately controlling a desired speed to a desired value.

In order to solve the above-mentioned problem, the present invention uses a vapor deposition source comprising a container for accommodating a vapor deposition material and a heating means for heating the container, and the container is heated from the container by heating the container with the heating means. A method for producing a vapor deposition film, wherein a vapor deposition film is formed on the substrate by discharging the evaporated vapor deposition material and depositing the vapor deposition material released on the substrate facing the container. Each step is executed.
(1) Deposition rate sensor placement step A deposition rate sensor with a shutter for measuring the deposition rate of the deposition material on the substrate is placed.
(2) Temperature sensor arrangement | positioning process The temperature sensor which measures the temperature of the said container is arrange | positioned.
(3) First Control Step A target deposition rate setting value set in advance while measuring the deposition rate by opening the shutter of the deposition rate sensor and attaching the deposition material released from the container to the deposition rate sensor. Feedback control is performed to manipulate the power supplied to the heating means so that the deviation from the measured deposition rate measurement value becomes small.
(4) Determination step In the first control step, it is determined whether or not the fluctuation amount of the deposition rate measurement value is within a predetermined range. If it is determined that the variation amount is within the predetermined range, the deposition rate is determined. The shutter of the sensor is closed and the first control process is interrupted.
(5) Second control step When it is determined in the determination step that the fluctuation amount of the deposition rate measurement value falls within a predetermined range, the temperature of the container at the time of the determination is set as a target temperature set value. Then, while measuring the temperature of the container with the temperature sensor, feedback control is performed to operate electric power supplied to the heating means so that a deviation between the target temperature setting value and the measured temperature measurement value becomes small. .
And the manufacturing method of the vapor deposition film which concerns on this invention performs the said 1st control process, the said determination process, and the said 2nd control process repeatedly in this order, after performing the said 2nd control process only for the predetermined time defined beforehand. It is characterized by.

According to the present invention, the vapor deposition rate sensor with the shutter is arranged in the vapor deposition rate sensor arranging step, and in the first control step, the deviation between the target vapor deposition rate setting value and the vapor deposition rate measured value is small with the shutter opened. Thus, feedback control is performed to manipulate the power supplied to the heating means.
In other words, except for using a deposition rate sensor with a shutter, as in the conventional deposition rate control method, feedback control is performed so that the measured deposition rate approaches the target deposition rate set value. Can be stabilized in a relatively short time.

  Further, according to the present invention, in the determination step, it is determined whether or not the fluctuation amount of the deposition rate measurement value is within a predetermined range, and when it is determined that it is within the predetermined range, The first control process is interrupted by closing the shutter. In a second control step described later, feedback control is performed with the shutter closed.

According to the present invention, the temperature sensor for measuring the temperature of the container is arranged in the temperature sensor arranging step, and the heating means is arranged so that the deviation between the target temperature set value and the temperature measured value becomes small in the second control step. Perform feedback control to manipulate the power supplied to the.
When depositing a metal material such as Ag, Mg, Al or the like, the inventors of the present invention will use a container when the deposition rate measurement value is stable (when the fluctuation amount of the deposition rate measurement value falls within a predetermined range). It was found that the temperature of was also stable. For this reason, when vapor-depositing the metal material as described above, if the temperature control value is feedback-controlled so as to approach the target temperature setting value in the second control step, the vapor deposition rate is not measured. Can be expected to approach the target deposition rate set value.

Further, according to the present invention, after the second control step is executed for a predetermined time, the first control step, the determination step, and the second control step are repeatedly executed in this order.
That is, feedback control (first control step) with the deposition rate sensor shutter open and feedback control (second control step) with the deposition rate sensor shutter closed are alternately and repeatedly executed. become. In the state where the shutter is closed, the vapor deposition material does not adhere to the vapor deposition rate sensor, so that the lifetime of the vapor deposition rate sensor can be extended as compared with the state where there is no shutter or the shutter is always opened. In addition, as described above, even in the second control step that does not use the measurement value of the vapor deposition rate sensor, it can be expected that the vapor deposition rate is controlled to approach the target vapor deposition rate setting value. The deposition rate can be stabilized for a long time by the control process.

As described above, according to the vapor deposition film manufacturing method of the present invention, the vapor deposition rate (deposition rate) can be accurately controlled to a desired value while extending the lifetime of the vapor deposition rate sensor.
The target temperature set value in the second control step of the present invention means the temperature of the container at the time when it is determined in the determination step that the fluctuation amount of the deposition rate measurement value is within the predetermined range. Can be exemplified by setting the temperature measurement value measured by the temperature sensor at the time point to the target temperature set value. Further, as described later, the temperature set value operated by the first feedback control at the time point can be set to the target temperature set value.

Here, in the first control step, the determination step, and the second control step, it is preferable to perform the following operations, respectively.
(A) 1st control process Opening the shutter of the said vapor deposition rate sensor, measuring the vapor deposition rate, and setting the temperature setting value of the said container so that the deviation of the said target vapor deposition rate setting value and the said vapor deposition rate measured value may become small At the same time as performing the first feedback control for operating the temperature sensor, the temperature sensor measures the temperature of the container, and the deviation between the temperature set value operated by the first feedback control and the measured temperature measurement value is small. Thus, the second feedback control for operating the power supplied to the heating means is performed.
(B) Determination step In the first control step, it is determined whether or not both of the fluctuation amount of the deposition rate measurement value and the fluctuation amount of the temperature measurement value are within a predetermined range, and within the predetermined range. If it is determined that it has fallen, the shutter of the vapor deposition rate sensor is closed and the first control step is interrupted.
(C) Second control step The temperature set value or the temperature at the time when it is determined in the determination step that both of the fluctuation amount of the deposition rate measurement value and the fluctuation amount of the temperature measurement value are within a predetermined range, respectively. A measured value is set as a target temperature set value, and the temperature of the container is measured by the temperature sensor and supplied to the heating means so that a deviation between the target temperature set value and the measured temperature measured value becomes small. Perform feedback control to control the power to be used.

According to the preferable configuration, in the first control step, the target vapor deposition rate setting is not directly operated so that the deviation between the target vapor deposition rate setting value and the vapor deposition rate measurement value is small, instead of directly operating the power supplied to the heating unit. The first feedback control for operating the temperature setting value of the container is performed so that the deviation between the value and the deposition rate measurement value is small, and the deviation between the temperature setting value and the temperature measurement value operated by the first feedback control is small. Thus, the second feedback control for operating the power supplied to the heating means is performed.
In other words, the feedback control using both the temperature setting value of the container and the power supplied to the heating means as the control amount is performed in cascade control, so that the deposition rate measurement value can be set more stably. It is possible to approach the value and to stabilize the temperature of the container.

According to the preferable configuration, in the determination step, it is determined whether both of the fluctuation amount of the deposition rate measurement value and the fluctuation amount of the temperature measurement value are within a predetermined range, and are within the predetermined range. If it is determined that it has been, the shutter of the deposition rate sensor is closed and the first control process is interrupted.
Further, according to the preferable configuration, in the second control step, at the time when it is determined that both the target temperature set value (the variation amount of the deposition rate measurement value and the variation amount of the temperature measurement value are within a predetermined range, respectively). The feedback control is performed to operate the electric power supplied to the heating means so that the deviation between the temperature setting value or the temperature measurement value) and the temperature measurement value becomes small.

  According to the preferred configuration, by performing cascade control in the first control step, it is easy to stabilize both the deposition rate measurement value and the temperature measurement value, and both the deposition rate measurement value and the temperature measurement value are stable. In order to execute the second control step after determining in the determination step, the deposition rate is further controlled to approach the target deposition rate set value without measuring the deposition rate in the second control step. I can expect.

In the method for producing a vapor deposition film according to the present invention, the base material is a long strip base material, the vapor deposition material is a metal vapor deposition material, and the base material is transported in the longitudinal direction on the base material. This is particularly effective when forming a deposited film.
In other words, it is particularly effective when applied to an object having a high vapor deposition rate and whose lifetime of the vapor deposition rate sensor is likely to decrease.

  In order to solve the above problems, the present invention provides a vapor deposition source including a container for storing a vapor deposition material and a heating means for heating the container, a power source for supplying power to the heating means, and a discharge from the vapor deposition source. A deposition rate sensor with a shutter that measures the deposition rate of the deposition material on the substrate, a temperature sensor that measures the temperature of the container, the power source, and the deposition rate sensor And a control means connected to the temperature sensor, wherein the control means controls a first control part, a determination part, a second control part, and an opening / closing operation of the shutter of the vapor deposition rate sensor, and A main control unit that controls operations of the first control unit, the determination unit, and the second control unit, the main control unit opens a shutter of the vapor deposition rate sensor, and the first control unit main In a state where the shutter of the vapor deposition rate sensor is opened by the control unit, the power source is set so that a deviation between a target vapor deposition rate setting value set and stored in advance and a vapor deposition rate measurement value input from the vapor deposition rate sensor is small Feedback control is performed to operate the power set value of, and during the feedback control by the first control unit, the determination unit determines whether or not the variation amount of the deposition rate measurement value is within a predetermined range, When the determination unit determines that the fluctuation amount of the deposition rate measurement value is within a predetermined range, the main control unit closes the shutter of the deposition rate sensor, and the second control unit The temperature of the container at the time of determining that the fluctuation amount of the deposition rate measurement value is within a predetermined range is set and stored as a target temperature setting value, and the target temperature setting value , Feedback control is performed to operate the power set value of the power supply so that a deviation from the temperature measurement value input from the temperature sensor is small, and the main control unit is configured to perform feedback control by the second control unit in advance. After being executed for a predetermined time, the shutter opening operation of the deposition rate sensor, the feedback control by the first control unit, the determination by the determination unit, the shutter closing operation of the deposition rate sensor, and the second control It is also provided as a vapor deposition apparatus characterized by repeatedly executing feedback control by the unit in this order.

  Preferably, the first control unit includes a first feedback control unit and a second feedback control unit, and the first feedback control unit has a shutter of the deposition rate sensor opened by the main control unit. At the same time, the second feedback control unit performs the feedback control for operating the temperature setting value of the container so that the deviation between the target deposition rate setting value and the deposition rate measurement value is small. 1 performing feedback control to operate the power setting value of the power supply so that a deviation between the temperature setting value operated by the feedback control unit and the temperature measurement value input from the temperature sensor is small; During the feedback control by the first control unit, the fluctuation amount of the deposition rate measurement value and the fluctuation amount of the temperature measurement value are both calculated. Are determined to be within a predetermined range, and the determination unit determines that both of the fluctuation amount of the deposition rate measurement value and the fluctuation amount of the temperature measurement value are within the predetermined range. The main control unit closes the shutter of the deposition rate sensor, and the second control unit determines that the determination unit has both a variation amount of the deposition rate measurement value and a variation amount of the temperature measurement value within a predetermined range. The temperature setting value at the time when it is determined that the temperature is within or the temperature measurement value input from the temperature sensor is set and stored as a target temperature setting value, and the target temperature setting value and the temperature measurement input from the temperature sensor are stored. Feedback control is performed to manipulate the power setting value of the power supply so that the deviation from the value becomes small.

  ADVANTAGE OF THE INVENTION According to this invention, a vapor deposition rate (film-forming speed | rate) is accurately controllable to the desired target value, extending the lifetime of the vapor deposition rate sensor which measures a vapor deposition rate by making vapor deposition material adhere.

FIG. 1 is a block diagram schematically showing a configuration of a control means in a conventional vapor deposition apparatus. FIG. 2 is a diagram schematically showing the overall configuration of the vapor deposition apparatus according to the embodiment of the present invention. FIG. 3 is a block diagram schematically showing the configuration of the control means in the vapor deposition apparatus according to the first embodiment of the present invention. FIG. 4 is a diagram schematically illustrating an example of a control result of the deposition rate by the deposition apparatus according to the first embodiment of the present invention. FIG. 5 is a block diagram schematically showing the configuration of the control means in the vapor deposition apparatus according to the second embodiment of the present invention. FIG. 6 is a diagram schematically illustrating an example of a deposition rate control result by the deposition apparatus according to the second embodiment of the present invention and an example of a deposition rate control result by the conventional deposition apparatus.

  Hereinafter, embodiments (first embodiment and second embodiment) of the present invention will be described with reference to the accompanying drawings as appropriate. First, the whole structure of the vapor deposition apparatus common to 1st Embodiment and 2nd Embodiment is demonstrated. In addition, the dimension of each part shown by each figure, such as thickness and length, and the reduced scale ratio of each part differ from an actual thing for convenience of illustration.

<Overall configuration of vapor deposition apparatus>
FIG. 2 is a diagram schematically showing the overall configuration of the vapor deposition apparatus according to the embodiment of the present invention.
As shown in FIG. 2, the vapor deposition apparatus 100 according to this embodiment includes a crucible 11 containing a vapor deposition material and a vapor deposition source 1 including a heating unit 12 for heating the crucible 11, and a power source for supplying power to the heating unit 12. 2 and the vapor deposition material released from the vapor deposition source 1 are attached, and the temperature of the vapor deposition rate sensor 3 with the shutter 31 for measuring the vapor deposition rate of the vapor deposition material on the substrate S and the temperature of the crucible 11 are measured. A temperature sensor 4, a power source 2, a vapor deposition rate sensor 3, and a control means 5 connected to the temperature sensor 4 are provided.

  Although it does not specifically limit as the heating means 12, For example, the wire heater using a metal wire, such as tungsten and a tantalum, an infrared lamp, etc. are used. When a wire heater is used, a metal wire is wound around the outer peripheral surface of the crucible 11, and power is supplied to the metal wire from the power source 2, whereby the metal wire and thus the crucible 11 is heated.

  The deposition rate sensor 3 is not particularly limited as long as it is a sensor that measures the deposition rate by attaching a deposition material, but a QCM sensor is preferably used. As a QCM sensor with a shutter, for example, a dual sensor manufactured by Infocon can be exemplified.

  Although it does not specifically limit as the temperature sensor 4, For example, a thermocouple is used. When a wire heater is used as the heating means 12, the temperature of the crucible 11 is measured by inserting a thermocouple between the outer peripheral surface of the crucible 11 and the wire heater.

  Although it does not specifically limit as the control means 5, For example, PLC (programmable logic controller) in which the program for performing the control method mentioned later (the function of each part with which the control means 5 is provided) was installed was installed. And PC (personal computer).

  The vapor deposition apparatus 100 according to the present embodiment includes a vacuum chamber 6 in which the inside is evacuated, and a transport device 7 that is disposed in the vacuum chamber 6 and transports the substrate S. The vapor deposition source 1 is disposed in the vacuum chamber 6 and is disposed to face the surface of the substrate S so that the vaporized vapor deposition material collides in a direction substantially orthogonal to the surface of the substrate S. For example, the vapor deposition source 1 is fixed to the bottom of the second chamber 62 described later.

  The substrate S is formed in a long band shape. The substrate S is an elongated rectangular flexible sheet. The length of the long belt-like substrate S (the length of the substrate S in the MD direction) is not particularly limited, but is, for example, 10 m or more, preferably 30 m or more, more preferably 50 m or more, The upper limit is, for example, 3000 m or less, preferably 2000 m or less, and more preferably 1000 m or less. Further, the width of the long belt-like substrate S (the length of the substrate S in the TD direction) is not particularly limited, but is, for example, 5 mm or more, preferably 8 mm or more, more preferably 10 mm or more, The upper limit is, for example, 500 mm or less, preferably 400 mm or less, and more preferably 300 mm or less.

The inside of the vacuum chamber 6 is partitioned into, for example, two chambers 61 and 62 (hereinafter referred to as a first chamber 61 and a second chamber 62) via a partition wall 63. The conveyance device 7 conveys the base material S to the vapor deposition area where the vapor deposition source 1 is disposed. The transport device 5 includes a first roll 71 arranged at a predetermined position in the first chamber 61, a can roll 73 arranged in the second chamber 62, and a second roll arranged at a predetermined position in the first chamber 61. And a roll 72. The second chamber 62 constitutes a vapor deposition area. The vacuum chamber 6 is provided with a vacuum pump (not shown). Moreover, you may provide the reactive gas supply apparatus (not shown) which supplies a reactive gas in the vacuum chamber 6 as needed.
In FIG. 2, a vapor deposition apparatus 100 (a roll-to-roll type vapor deposition apparatus) that deposits a vapor deposition material on the base material S while the long strip-shaped base material S is wound up from the first roll 71 to the second roll 72. 100).
Moreover, the vacuum chamber 6 is not limited to the case where the vacuum chamber 6 is partitioned into two chambers of the first chamber 61 and the second chamber 62, and may be configured by one chamber, or may be partitioned into three or more chambers. May be.

  The base material S fed out from the first roll 71 is conveyed in the longitudinal direction (downstream in the MD direction), passes through the vapor deposition area of the second chamber 62 while being in contact with the surface of the can roll 73, and then the second roll. 72 is wound up. While the base material S passes the surface (evaporation area) of the can roll 73, the vapor deposition material released from the vapor deposition source 1 is deposited, and a vapor deposition film (thin film) is formed on the surface of the base material S. . In addition, the arrow shown in FIG. 2 shows the conveyance direction of the base material S. FIG.

  The distance between the upper end portion of the vapor deposition source 1 (the upper end portion of the nozzle that discharges the vapor deposition material) and the surface of the substrate S can be set as appropriate, but is, for example, 0.2 mm to 5 mm, preferably 0.5 mm to 4 mm. It is. By installing the vapor deposition source 1 so as to have such a distance, the vapor deposition apparatus 100 having a high vapor deposition rate can be configured. The vapor deposition apparatus 100 having a high vapor deposition rate can continuously form a vapor deposition film having a desired thickness on the long belt-like substrate S.

The substrate S is not particularly limited as long as it is a flexible sheet-like material. For example, a resin sheet such as polyethylene naphthalate or polyimide; a metal foil or metal sheet such as stainless steel (SUS); a glass sheet; Can do.
The conveyance speed of the base material S is 0.5 m / min or more, for example, Preferably, it is 1 m / min-20 m / min.
Degree of vacuum in the vacuum chamber 6, for example, not more than 1 × ¹⁰ -3 Pa, preferably ^{1 × 10 -5 Pa~1 × 10 -3} Pa.
The vapor deposition material put into the crucible 11 of the vapor deposition source 1 can be appropriately selected according to the vapor deposition film to be formed. The heating temperature (target temperature setting value) of the crucible 11 of the vapor deposition source 1 is appropriately set according to the vapor deposition material.

  2 illustrates a configuration in which one deposition source 1 is arranged in one vacuum chamber 6, but the deposition apparatus according to the present invention has two or more deposition sources arranged in one vacuum chamber. A configuration is also possible. Moreover, the vapor deposition apparatus according to the present invention can be configured to include two or more vacuum chambers in which vapor deposition sources are arranged. Thus, by using a vapor deposition apparatus in which two or more vapor deposition sources are arranged in one vacuum chamber or a vapor deposition apparatus having two or more vacuum chambers in which vapor deposition sources are arranged, different types of vapor deposition materials can be continuously used. Vapor deposition can be performed, and different types of deposited films can be formed on top of each other.

The vapor deposition apparatus 100 which concerns on this embodiment can be used for formation of various thin films (vapor deposition film). Preferably, it is used for forming a metal film such as an electrode film of an organic EL element. However, the present invention is not limited to this, an organic film of an organic EL element, a semiconductor layer of a thin film transistor (TFT), a photoelectric conversion layer in a photovoltaic element such as a thin film solar cell, a semiconductor light emitting layer in an organic light emitting diode or an organic light emitting transistor, etc. It can be used for forming various thin films such as (organic TFT layer).
When forming an electrode film of an organic EL element, for example, indium tin oxide (ITO); indium tin oxide containing silicon oxide (ITSO); aluminum; gold; platinum; nickel; tungsten; copper; Silver; magnesium; alloy; zinc oxide added with a conductive metal such as aluminum (ZnO: Al); magnesium-silver alloy.

  The vapor deposition apparatus 100 having the overall configuration described above is characterized by a method for controlling the vapor deposition rate. Hereinafter, the first embodiment and the second embodiment, which are different in control method (the configuration of the control means 5 is different), will be sequentially described.

<First Embodiment>
FIG. 3 is a block diagram schematically showing the configuration of the control means in the vapor deposition apparatus according to the first embodiment of the present invention.
As shown in FIG. 3, the control means 5 included in the vapor deposition apparatus 100 according to the first embodiment includes a first control unit 51, a determination unit 52, a second control unit 53, and a shutter 31 of the vapor deposition rate sensor 3. A main control unit 54 that controls the opening / closing operation and the operations of the first control unit 51, the determination unit 52, and the second control unit is provided.
The following first control step, determination step, and second control step are sequentially executed by the control means 5 having the configuration described above.

(First control process)
In the first control step, first, the main control unit 54 opens the shutter 31 of the deposition rate sensor 3 (moves the shutter 31 to the position indicated by the broken line in FIG. 3). Thereby, the vapor deposition material discharged | emitted from the crucible 11 adheres to the vapor deposition rate sensor 3, and a vapor deposition rate can be measured.
Next, in a state where the shutter 31 of the deposition rate sensor 3 is opened by the main control unit 54, the first control unit 51 and the target deposition rate set value SV1 set and stored in advance and the deposition input from the deposition rate sensor 3 are performed. Feedback control (for example, PID control) for operating the power setting value MV2 of the power supply 2 is performed so that the deviation from the rate measurement value PV1 becomes small. Thereby, the power supply 2 supplies the electric power according to the electric power setting value MV2 to the heating means 12.

(Judgment process)
In the determination step, the determination unit 52 determines whether or not the fluctuation amount of the deposition rate measurement value PV1 falls within a predetermined range in the first control step (during feedback control by the first control unit 51). The fluctuation amount of the deposition rate measurement value PV1 is evaluated by, for example, a CV value (coefficient of variation) represented by a value obtained by dividing the standard deviation of the deposition rate measurement value PV1 within a predetermined time by an average value. And the difference between the deposition rate measured value PV1 and the target deposition rate set value SV1 within a predetermined time is within a predetermined range with respect to the target deposition rate set value SV1 (for example, the target deposition rate If both of them are within the range of ± 5% of the set value SV1, it is possible to determine that the fluctuation amount of the deposition rate measured value PV1 is within the predetermined range.
When the determination unit 52 determines that the fluctuation amount of the deposition rate measurement value PV1 is within a predetermined range, the main control unit 54 closes the shutter 31 of the deposition rate sensor 3 (at a position indicated by a solid line in FIG. 3). The shutter 31 is moved). Thereby, the first control process is interrupted.

(Second control process)
In the second control step, first, the second control unit 53 sets the temperature of the crucible 11 at the time when the determination unit 52 determines that the fluctuation amount of the deposition rate measurement value PV1 falls within a predetermined range. The setting is stored as a set value. Specifically, the temperature measurement value PV2 measured by the temperature sensor 4 at the time point is input to the second control unit 53, and the input temperature measurement value PV2 is set and stored in the second control unit 53 as the target temperature setting value. Is done.
Next, the second control unit 53 operates feedback control (operating the power set value MV2 of the power source 2 so that the deviation between the target temperature set value and the temperature measured value PV2 input from the temperature sensor 4 becomes small). For example, PID control) is performed. As a result, the power source 2 supplies power corresponding to the power set value MV2 to the heating unit 12.

  The main control unit 54 performs the first control step, the determination step, and the second control step after the second control step (feedback control by the second control unit 53) is executed for a predetermined time. The processes are repeated in this order until the formation of the deposited film on the material S is completed. That is, the opening operation of the shutter 31 of the deposition rate sensor 3, the feedback control by the first control unit 51, the determination by the determination unit 52, the closing operation of the shutter 31 of the deposition rate sensor 3, and the feedback control by the second control unit 53. Repeat in order.

  The vapor deposition apparatus 100 according to the first embodiment including the control means 5 that performs the operation described above vapor-deposits a vapor deposition material that stabilizes the temperature measurement value PV2 of the crucible 11 when the vapor deposition rate measurement value PV1 is stable. It is effective when

FIG. 4 is a diagram schematically illustrating an example of a deposition rate control result by the deposition apparatus 100 according to the first embodiment. FIG. 4 shows an example in which the first control process, the determination process, and the second control process are each performed only once, but in practice, these are repeatedly performed.
In the example shown in FIG. 4, the shutter 31 of the vapor deposition rate sensor 3 is opened to start vapor deposition, and the power setting value MV2 of the power source 2 is set so that the deviation between the target vapor deposition rate setting value SV1 and the vapor deposition rate measurement value PV1 becomes small. Feedback control is performed (first control step).
Then, in the first control step, it is determined whether or not the fluctuation amount of the deposition rate measured value PV1 is within a predetermined range. If it is determined that the fluctuation amount is within the predetermined range, the shutter 31 of the deposition rate sensor 3 is closed. The first control process is interrupted (determination process). As can be seen from FIG. 4, when the shutter 31 of the deposition rate sensor 3 is closed, the temperature measurement value PV2 of the crucible 11 is also stable.
For this reason, the temperature measurement value PV2 of the crucible 11 at the time point is set as a target temperature setting value, and the power setting of the power source 2 is set so that the deviation between the target temperature setting value and the temperature measurement value PV2 by the temperature sensor 4 is small. Also by performing feedback control (PID control) for manipulating the value MV2 (second control step), the deposition rate measured value PV1 can be controlled to approach the target deposition rate set value SV1.
The execution of the determination step can be started simultaneously with the start of the execution of the first control step, but may be started after a predetermined time has elapsed since the start of the execution of the first control step.

Second Embodiment
FIG. 5 is a block diagram schematically showing the configuration of the control means in the vapor deposition apparatus according to the second embodiment of the present invention.
As shown in FIG. 5, the control means 5 included in the vapor deposition apparatus 100 according to the second embodiment is similar to the first embodiment in that the first control unit 51, the determination unit 52, the second control unit 53, While controlling the opening / closing operation | movement of the shutter 31 of the vapor deposition rate sensor 3, the main control part 54 which controls the operation | movement of the 1st control part 51, the determination part 52, and the 2nd control part is comprised. However, unlike the first embodiment, the first control unit 51 of the second embodiment includes a first feedback control unit 511 and a second feedback control unit 512.
The following first control step, determination step, and second control step are sequentially executed by the control means 5 having the configuration described above.

(First control process)
In the first control step, first, the main control unit 54 opens the shutter 31 of the vapor deposition rate sensor 3, and the first feedback control unit 511 opens the shutter 31 of the vapor deposition rate sensor 3 by the main control unit 54. In this state, the first feedback for operating the temperature setting value SV2 of the crucible 11 so that the deviation between the target deposition rate setting value SV1 set and stored in advance and the deposition rate measured value PV1 input from the deposition rate sensor 3 becomes small. Control (for example, PID control) is performed. At the same time, the second feedback control unit 512 controls the power supply 2 so that the deviation between the temperature set value SV2 operated by the first feedback control unit 511 and the temperature measurement value PV2 input from the temperature sensor 4 becomes small. Second feedback control (for example, PID control) for operating the power set value MV2 is performed. Thereby, the power supply 2 supplies the electric power according to the electric power setting value MV2 to the heating means 12.

(Judgment process)
In the determination step, the determination unit 52 determines that both the fluctuation amount of the deposition rate measurement value PV1 and the fluctuation amount of the temperature measurement value PV2 are in a predetermined range in the first control step (during feedback control by the first control unit 51). It is determined whether or not it is within. As for the fluctuation amount of the deposition rate measurement value PV1, as in the first embodiment, the CV value is equal to or less than a predetermined threshold, and the deposition rate measurement value PV1 and the target deposition rate set value SV1 within a predetermined time. Of the deposition rate measured value PV1 is satisfied if both of the above are within a predetermined range with respect to the target deposition rate set value SV1 (for example, within ± 5% of the target deposition rate set value SV1). It is possible to determine that the fluctuation amount is within a predetermined range. The fluctuation amount of the temperature measurement value PV2 is evaluated by, for example, a CV value. If the CV value is equal to or less than a predetermined threshold value, it is determined that the fluctuation amount of the temperature measurement value PV2 is within a predetermined range. Is possible.
When the determination unit 52 determines that both the fluctuation amount of the vapor deposition rate measurement value PV1 and the fluctuation amount of the temperature measurement value PV2 are within the predetermined ranges, the main control unit 54 selects the shutter of the vapor deposition rate sensor 3. 31 is closed. Thereby, the first control process is interrupted.

(Second control process)
In the second control step, first, the second control unit 53 determines that the determination unit 52 determines that both the fluctuation amount of the deposition rate measurement value PV1 and the fluctuation amount PV2 of the temperature measurement value are within a predetermined range. The temperature setting value SV2 or the temperature measurement value PV2 at the time point is set and stored as the target temperature setting value. When the temperature set value SV2 is set as the target temperature set value, the temperature set value SV2 input to the second feedback control unit 512 is input to the second control unit 53 via the main control unit 54, and this input The temperature set value SV2 is set and stored in the second control unit 53 as the target temperature set value.
Next, the second control unit 53 operates feedback control (operating the power set value MV2 of the power source 2 so that the deviation between the target temperature set value and the temperature measured value PV2 input from the temperature sensor 4 becomes small). For example, PID control) is performed. Thereby, the power supply 2 supplies the electric power according to the electric power setting value MV2 to the heating means 12.

  The main control unit 54 performs the first control step, the determination step, and the second control step after the second control step (feedback control by the second control unit 53) is executed for a predetermined time. The processes are repeated in this order until the formation of the deposited film on the material S is completed. That is, the opening operation of the shutter 31 of the deposition rate sensor 3, the feedback control by the first control unit 51, the determination by the determination unit 52, the closing operation of the shutter 31 of the deposition rate sensor 3, and the feedback control by the second control unit 53. Repeat in order.

  The vapor deposition apparatus 100 according to the second embodiment including the control means 5 that performs the operation described above operates both the temperature set value SV2 of the crucible 11 and the power set value MV2 of the power source 2 in the first control step. Since the feedback control for the quantity is cascade control with a double loop, the deposition rate measurement value PV1 can be made more stable and close to the target deposition rate set value SV1, and the temperature measurement value PV2 of the crucible 11 is also stable. It is possible to make it.

FIG. 6 shows an example of a deposition rate control result (FIG. 6A) by the deposition apparatus 100 according to the second embodiment of the present invention and an example of a deposition rate control result by the conventional deposition apparatus (FIG. 1) (FIG. 6). 6 (b)) is a diagram schematically showing. FIG. 6A shows an example in which the second control step is executed only once, but in practice, the first control step, the determination step, and the second control step are repeatedly executed.
In the example shown in FIG. 6A, the temperature of the crucible 11 is set so that the shutter 31 of the vapor deposition rate sensor 3 is opened and vapor deposition is started, and the deviation between the target vapor deposition rate setting value SV1 and the vapor deposition rate measurement value PV1 becomes small. At the same time as performing the first feedback control (PID control) for manipulating the set value SV2, the second feedback for manipulating the power set value MV2 of the power source 2 so that the deviation between the temperature set value SV2 and the temperature measured value PV2 becomes small. Control (PID control) is performed (first control step).
Then, in the first control step, it is determined whether both of the fluctuation amount of the deposition rate measurement value PV1 and the fluctuation amount of the temperature measurement value PV2 are within a predetermined range, and it is determined that they are within the predetermined range. In this case, the shutter 31 of the deposition rate sensor 3 is closed and the first control process is interrupted (determination process). As can be seen from FIG. 6A, when the shutter 31 of the vapor deposition rate sensor 3 is closed, both the vapor deposition rate measurement value PV1 and the temperature measurement value PV2 are stabilized by performing cascade control in the first control step. ing.
Next, the temperature setting value SV2 or the temperature measurement value PV2 at the time point is set as the target temperature setting value, and the power supply 2 is set so that the deviation between the target temperature setting value and the temperature measurement value PV2 by the temperature sensor 4 is small. Feedback control (PID control) for operating the power set value MV2 is performed (second control step). Thereby, it can control so that vapor deposition rate measured value PV1 approaches target vapor deposition rate setting value SV1.
As in the first embodiment, the execution of the determination step can be started simultaneously with the start of the execution of the first control step, but a predetermined time has elapsed since the start of the execution of the first control step. You may start later.

On the other hand, as can be seen from FIG. 6B, the power setting value MV2 of the power source 2 is set to be controlled by the conventional vapor deposition apparatus (simply, the deviation between the target vapor deposition rate setting value SV1 and the vapor deposition rate measurement value PV1 is small) In the control to operate, the deposition rate measurement value PV1 can be stabilized, but the temperature measurement value PV2 and the power set value MV2 cannot be stabilized. For this reason, even if the vapor deposition rate sensor 3 with the shutter 31 is used to extend the lifetime of the vapor deposition rate sensor 3, after the shutter 31 is closed, the feedback using the temperature measurement value PV2 and the power set value MV2 is used. Control cannot be performed.
On the other hand, the vapor deposition apparatus 100 according to the second embodiment can stabilize both the vapor deposition rate measured value PV1 and the temperature measured value PV2 by performing cascade control in the first control step. After closing, it is possible to perform feedback control using the temperature measurement value PV2 in the second control step.

DESCRIPTION OF SYMBOLS 1 ... Deposition source 2 ... Power supply 3 ... Deposition rate sensor 4 ... Temperature sensor 5 ... Control means 11 ... Container 12 ... Heating means 31 ... Shutter 100 ... Vapor deposition device S ... Base material

Claims (5)

By using a vapor deposition source comprising a container for storing the vapor deposition material and a heating means for heating the container, the vaporization material evaporated from the container is discharged by heating the container with the heating means, A method for producing a vapor deposition film, in which a vapor deposition film is formed on the substrate by depositing the vapor deposition material released on an opposing substrate,
A deposition rate sensor placement step of placing a deposition rate sensor with a shutter for measuring a deposition rate of the deposition material on the substrate;
A temperature sensor arrangement step of arranging a temperature sensor for measuring the temperature of the container;
While measuring the vapor deposition rate by opening the shutter of the vapor deposition rate sensor and attaching the vapor deposition material released from the container to the vapor deposition rate sensor, the target vapor deposition rate set value and the measured vapor deposition rate measured value are set in advance. A first control step for performing feedback control for operating the power supplied to the heating means so that the deviation from
In the first control step, it is determined whether or not the fluctuation amount of the deposition rate measurement value falls within a predetermined range. If it is determined that the variation amount falls within the predetermined range, the shutter of the deposition rate sensor is closed. Determining step for interrupting the first control step;
In the determination step, when it is determined that the fluctuation amount of the deposition rate measurement value is within a predetermined range, the temperature of the container at the time of the determination is set as a target temperature setting value, and the temperature sensor A second control step of performing feedback control for operating electric power supplied to the heating means so that a deviation between the target temperature setting value and the measured temperature measurement value is reduced while measuring the temperature of the container And
After executing the second control step for a predetermined time, the first control step, the determination step, and the second control step are repeatedly executed in this order.
The manufacturing method of the vapor deposition film characterized by the above-mentioned. In the first control step, the temperature setting value of the container is set so that a deviation between the target deposition rate setting value and the deposition rate measurement value becomes small while opening the shutter of the deposition rate sensor and measuring the deposition rate. At the same time as performing the first feedback control for operating the temperature sensor, the temperature sensor measures the temperature of the container, and the deviation between the temperature set value operated by the first feedback control and the measured temperature measurement value is small. And performing a second feedback control for operating the power supplied to the heating means,
In the determination step, in the first control step, it is determined whether both of the fluctuation amount of the deposition rate measurement value and the fluctuation amount of the temperature measurement value are within a predetermined range, and within the predetermined range. If it is determined that it has fallen, the first control step is interrupted by closing the shutter of the vapor deposition rate sensor,
In the second control step, the temperature set value or the temperature at the time when it is determined in the determination step that both the fluctuation amount of the deposition rate measurement value and the fluctuation amount of the temperature measurement value are within a predetermined range, respectively. A measured value is set as a target temperature set value, and the temperature of the container is measured by the temperature sensor and supplied to the heating means so that a deviation between the target temperature set value and the measured temperature measured value becomes small. Perform feedback control to manipulate the power to
The manufacturing method of the vapor deposition film of Claim 1 characterized by the above-mentioned. The base material is a long belt-like base material,
The vapor deposition material is a metal vapor deposition material,
Forming a vapor deposition film on the substrate while conveying the substrate in the longitudinal direction;
The manufacturing method of the vapor deposition film of Claim 1 or 2 characterized by the above-mentioned. A vapor deposition source comprising a container containing a vapor deposition material and a heating means for heating the container;
A power supply for supplying power to the heating means;
A deposition rate sensor with a shutter that measures the deposition rate of the deposition material on the substrate by attaching the deposition material released from the deposition source;
A temperature sensor for measuring the temperature of the container;
Control means connected to the power source, the vapor deposition rate sensor and the temperature sensor;
The control means controls a first control unit, a determination unit, a second control unit, and an opening / closing operation of a shutter of the vapor deposition rate sensor, and the first control unit, the determination unit, and the second control unit. A main control unit for controlling the operation of
The main control unit opens a shutter of the deposition rate sensor,
The first control unit includes a target deposition rate setting value set and stored in advance in a state where the shutter of the deposition rate sensor is opened by the main control unit, and a deposition rate measurement value input from the deposition rate sensor. Perform feedback control to manipulate the power setting value of the power supply so that the deviation is small,
The determination unit determines whether or not the fluctuation amount of the deposition rate measurement value falls within a predetermined range during the feedback control by the first control unit,
When the determination unit determines that the variation amount of the deposition rate measurement value is within a predetermined range, the main control unit closes the shutter of the deposition rate sensor,
The second control unit sets and stores the temperature of the container as a target temperature setting value when the determination unit determines that the fluctuation amount of the deposition rate measurement value falls within a predetermined range, and the target temperature setting Feedback control is performed to manipulate the power setting value of the power supply so that the deviation between the value and the temperature measurement value input from the temperature sensor is small,
The main control unit, after the feedback control by the second control unit is executed for a predetermined time, the shutter opening operation of the deposition rate sensor, the feedback control by the first control unit, the determination by the determination unit , Repeatedly performing the shutter closing operation of the deposition rate sensor and the feedback control by the second control unit in this order,
The vapor deposition apparatus characterized by the above-mentioned. The first control unit includes a first feedback control unit and a second feedback control unit, and the first feedback control unit is in a state where a shutter of the deposition rate sensor is opened by the main control unit, At the same time as performing feedback control to manipulate the temperature setting value of the container so that the deviation between the target deposition rate setting value and the deposition rate measurement value is small, the second feedback control unit is configured to perform the first feedback control. Feedback control is performed to operate the power setting value of the power supply so that the deviation between the temperature setting value operated by the unit and the temperature measurement value input from the temperature sensor is small,
The determination unit determines whether both of the fluctuation amount of the deposition rate measurement value and the fluctuation amount of the temperature measurement value are within a predetermined range during feedback control by the first control unit,
When the determination unit determines that both the variation amount of the deposition rate measurement value and the variation amount of the temperature measurement value are within a predetermined range, the main control unit closes the shutter of the deposition rate sensor,
The second control unit is configured such that the temperature setting value or the temperature when the determination unit determines that both of the fluctuation amount of the deposition rate measurement value and the fluctuation amount of the temperature measurement value are within a predetermined range, respectively. The temperature measurement value input from the sensor is set and stored as a target temperature setting value, and the power setting value of the power supply is set so that the deviation between the target temperature setting value and the temperature measurement value input from the temperature sensor is small. Perform feedback control to operate,
The vapor deposition apparatus of Claim 4 characterized by the above-mentioned.

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