JP6116290B2 - Vapor deposition apparatus and vapor deposition method - Google Patents

Description

  The present invention relates to a vapor deposition apparatus used for vapor deposition of metal thin films, organic material thin films, metal electrode wirings such as solar cells and display panels, and organic EL light emitting layers, and a vapor deposition method using the apparatus.

In general, the thin film and the like are formed under a high vacuum of 10 ⁻⁴ Pa or less. For example, as shown in Patent Document 1, a vacuum deposition apparatus includes a dispersion container (manifold) in which a vapor deposition material (evaporation material) evaporated from a material storage container (crucible) provided with a heating mechanism is introduced in a vacuum chamber. The evaporating material is discharged from a plurality of nozzles provided on the upper part of the manifold and deposited on the substrate to form a thin film. This vapor deposition apparatus can obtain film thickness uniformity for a large-area substrate even if there is no movable part such as substrate rotation by optimizing the nozzle design (arrangement, size, angle, etc.) of the manifold. Has the advantage.

  Usually, the amount of evaporation material deposited per unit time on the substrate, that is, the deposition rate is controlled by the heating temperature of the crucible, but the temperature is gradually transferred to the deposition material in the crucible by heat conduction, etc. The rate is difficult to stabilize. Therefore, there is a method of stabilizing the vapor deposition rate by inserting a flow rate adjusting valve in the path of the evaporated molecules and feeding back a signal from the film thickness sensor to the flow rate adjusting valve (for example, Patent Document 2).

  Quartz crystal type film thickness sensors are widely used as the film thickness sensors for the deposition rate measurement and the deposition rate control feedback. The crystal oscillator type film thickness sensor utilizes a phenomenon in which an AC electric field is applied to the crystal oscillator and resonates when the natural frequency of the crystal oscillator becomes equal to the frequency of the AC electric field. When a material such as a metal is deposited on the surface of the crystal unit, the natural frequency of the crystal unit changes in the direction of a low frequency. This amount of change is proportional to the amount n of the vapor deposition material. That is, the film thickness of the deposited material is calculated by accurately detecting the change in the resonance frequency using the resonance phenomenon described above.

  However, if a deposited film having a thickness of, for example, 7000 to 8000 angstroms (700 to 800 nm) is deposited on the surface of the crystal unit, the resonance frequency becomes low and the measurement error becomes large. Becomes difficult and must be replaced with a new crystal unit. For example, if the film formation process is performed at a deposition rate of 2 angstroms per minute (0.2 nm), the life of the crystal unit will be exhausted in about 60 to 70 hours. In this case, it is necessary to cool the evaporation source and return the inside of the vacuum chamber to atmospheric pressure. However, continuous vapor deposition for about one week is required in production lines and the like, and the vapor deposition material cannot be cooled frequently. For example, when the vapor deposition material is an organic compound for organic EL, vapor deposition is performed by heating to about 300 ° C. using a ceramic crucible or the like, but it takes several hours to cool and heat the crucible again. Therefore, since the vapor deposition process in the meantime stops, productivity falls.

  Therefore, Patent Document 3 discloses a vapor deposition apparatus that controls the vapor deposition rate without using a crystal resonator. In the vapor deposition apparatus disclosed in Patent Document 3, a crucible is disposed in a vacuum vessel, and a substrate holder is disposed opposite to the crucible. An electric heater is wound around the outer periphery of the crucible as a heating means for heating and evaporating the vapor deposition material accommodated in the crucible, and for measuring the pressure of the ambient atmosphere of the vapor deposition material in the vacuum vessel. A pressure sensor is arranged, a controller is connected to the pressure sensor, and an electric heater is connected to the controller.

  With this configuration, when electric power is supplied from the controller to the electric heater and the vapor deposition material in the crucible is heated by the electric heater, the pressure in the ambient atmosphere of the vapor deposition material is increased by the vaporized material released from the crucible, and is measured by the pressure sensor. Is done. Here, since there is a certain correlation between the pressure of the ambient atmosphere of the deposition material and the flow rate of the evaporation material, and there is also a certain correlation between the flow rate of the evaporation material and the deposition rate, the controller The vapor deposition rate can be calculated from the pressure measured by the pressure sensor. Therefore, the controller adjusts the current value supplied to the electric heater so that the pressure (measured value) measured by the pressure sensor becomes a preset value, thereby maintaining a predetermined vapor deposition rate. The thickness of the deposited film formed on the surface of the substrate is controlled.

JP 2005-330537 A JP 2010-242202 A JP 2004-91858 A

However, in Patent Document 3, the flow rate of the evaporation material is obtained using a single pressure sensor that measures the pressure of the ambient atmosphere of the vapor deposition material. This is thought to be because the pressure around the substrate is treated as a constant value, assuming that the pressure fluctuation around the substrate is small, but in reality, when the evaporation material is released into the vacuum chamber, the evaporation in the vacuum chamber Since the amount of material increases and pressure fluctuations occur, it cannot be said that the flow rate of the evaporation material can be measured, and a deposition film cannot be formed at an accurate deposition rate, and a desired film thickness is obtained. There was a problem that I could not.
In addition, with one pressure sensor, when a vapor deposition film is formed by co-evaporation using two types of vapor deposition materials, there is a problem in that the vapor deposition rate of each evaporation material cannot be obtained.

Therefore, the present invention can continuously measure the deposition rate without returning the vacuum chamber to the atmospheric pressure, can avoid a decrease in productivity, can accurately determine the flow rate of the evaporation material, and can accurately determine the deposition rate. An object of the present invention is to provide a vapor deposition apparatus and a vapor deposition method capable of forming a vapor deposition film.
In addition, the present invention can continuously measure the deposition rate without returning the vacuum chamber to atmospheric pressure, can avoid a decrease in productivity, and when forming a deposition film with two kinds of deposition materials, An object of the present invention is to provide a vapor deposition apparatus and a vapor deposition method that can accurately determine the flow rate and can form a vapor deposition film at an accurate vapor deposition rate.

The invention according to claim 1 of the present invention is
In a vacuum chamber, a vapor deposition apparatus for attaching an evaporation material to a vapor deposition member,
An evaporation source for storing the evaporation material and heating the evaporation material to obtain the evaporation material;
A guide path for transferring the evaporation material obtained in the evaporation source;
A discharge member that discharges the evaporating material flowing from the guide path to the deposition target member;
A flow rate control valve for adjusting the flow rate of the evaporation material supplied from the evaporation source to the induction path;
A first pressure sensor for detecting the pressure in the evaporation source;
A second pressure sensor for detecting the pressure in the vacuum chamber;
By measuring the flow rate of the evaporating material based on the difference between the value measured by the first pressure sensor and the value measured by the second pressure sensor, the evaporating rate of the evaporating material to the vapor deposition member is measured and measured. A controller for controlling the opening degree of the flow rate control valve so that the deposited deposition rate becomes a predetermined deposition rate;
It is provided with.

The invention according to claim 2 is the invention according to claim 1,
A discharge member includes a dispersion container for diffusing the evaporation material, and a plurality of nozzle members protruding toward the deposition target member and having a throttle opening at the tip for discharging the evaporation material to the deposition target member. It is characterized by having.

The invention described in claim 3
In a vacuum chamber, a vapor deposition apparatus for adhering a third vaporized material, which is a mixture of a first vaporized material and a second vaporized material having a smaller vapor deposition amount than the first vaporized material, to a vapor deposition member,
A first evaporation source containing the first evaporation material and heating the first evaporation material to obtain the first evaporation material;
A second evaporation source containing the second evaporation material and heating the second evaporation material to obtain the second evaporation material;
A first induction path for transferring the first evaporation material obtained in the first evaporation source;
A second induction path for transferring the second evaporation material obtained in the second evaporation source;
A third induction path for transferring the third evaporation material in which the first evaporation material and the second evaporation material are mixed by joining the first induction path and the second induction path;
A discharge member that discharges the third evaporation material flowing from the third guide path to the deposition target member;
A first flow rate control valve for adjusting a flow rate of the first evaporation material supplied from the first evaporation source to the first induction path;
A second flow rate control valve for adjusting a flow rate of the second evaporation material supplied from the second evaporation source to the second induction path;
A first pressure sensor for detecting the pressure in the first evaporation source;
A second pressure sensor for detecting the pressure in the vacuum chamber;
A third pressure sensor for detecting the pressure in the second evaporation source;
A fourth pressure sensor for detecting the pressure in the second guiding path;
The first deposition of the first evaporation material onto the vapor deposition member is obtained by determining the flow rate of the first evaporation material based on the difference between the value measured by the first pressure sensor and the value measured by the second pressure sensor. A rate is measured, the opening of the first flow rate control valve is controlled so that the measured first deposition rate becomes a predetermined first deposition rate, and the value measured by the third pressure sensor; By determining the flow rate of the second evaporation material based on the difference from the value measured by the pressure sensor, the second evaporation rate of the second evaporation material to the evaporation target member is measured, and the measured second evaporation rate is A controller for controlling the opening of the second flow rate control valve so as to achieve a predetermined second deposition rate;
It is provided with.

The invention according to claim 4 is the invention according to claim 3,
The release member is
A dispersion vessel for diffusing the third evaporation material;
A plurality of nozzle members protruding toward the vapor deposition member and having a throttle opening at the tip for releasing the third evaporation material to the vapor deposition member;
It is characterized by having.

The invention according to claim 5 is the invention according to claim 3 or 4,
A plurality of second evaporation sources and second induction paths;
A second flow rate control valve, a third pressure sensor, and a fourth pressure sensor are provided for each second evaporation source and second induction path,
The second vapor deposition materials stored in the respective second evaporation sources are different from each other.

Invention of Claim 6 is the vapor deposition method using the vapor deposition apparatus of Claim 1, Comprising:
Heating the vapor deposition material in an evaporation source to obtain the evaporation material;
Transferring the evaporation material obtained in the evaporation source into the induction path;
Discharging the evaporation material from the guide path through the discharge member to the deposition target member;
Adjusting the flow rate of the evaporation material supplied from the evaporation source to the induction path using the flow rate control valve;
Detecting the pressure in the evaporation source using the first pressure sensor;
Detecting a pressure in the vacuum chamber using a second pressure sensor;
Using the controller, the flow rate of the evaporating material is obtained based on the difference between the value measured by the first pressure sensor and the value measured by the second pressure sensor, and the evaporating material is obtained based on the obtained flow rate of the evaporating material. Measuring a deposition rate on the deposition target member, and controlling the opening of the flow rate control valve so that the measured deposition rate becomes a predetermined deposition rate;
It is characterized by including.

Invention of Claim 7 is the vapor deposition method using the vapor deposition apparatus of Claim 3, Comprising:
Heating the first vapor deposition material in the first evaporation source to obtain the first evaporation material;
Heating the second vapor deposition material in the second evaporation source to obtain the second evaporation material;
Transferring the first evaporation material obtained in the first evaporation source into the first induction path;
Transferring the second evaporation material obtained in the second evaporation source into the second induction path;
Transferring the third evaporating material in which the first evaporating material and the second evaporating material are mixed into the third guiding path by joining the first guiding path and the second guiding path;
Discharging the third evaporating material from the third guide path to the deposition target member via the release member;
Adjusting the flow rate of the first evaporation material supplied from the first evaporation source to the first induction path using the first flow rate control valve;
Adjusting the flow rate of the second evaporation material supplied from the second evaporation source to the second induction path using the second flow rate control valve;
Detecting the pressure in the first evaporation source using the first pressure sensor;
Detecting a pressure in the vacuum chamber using a second pressure sensor;
Detecting a pressure in the second evaporation source using a third pressure sensor;
Detecting a pressure in the second taxiway using a fourth pressure sensor;
Using the controller
A flow rate of the first evaporating material is obtained based on a difference between a value measured by the first pressure sensor and a value measured by the second pressure sensor, and the first evaporating material is obtained based on the obtained flow rate of the first evaporating material. The first deposition rate of the material to the deposition target member is measured, the opening of the first flow rate control valve is controlled such that the measured first deposition rate becomes a predetermined first deposition rate, and the third pressure The flow rate of the second evaporating material is obtained based on the difference between the value measured by the sensor and the value measured by the fourth pressure sensor, and the second evaporative material coating is obtained based on the obtained flow rate of the second evaporating material. Measuring a second deposition rate on the deposition member, and controlling the opening of the second flow rate control valve so that the measured second deposition rate becomes a predetermined second deposition rate;
It is characterized by including.

  According to the present invention, the deposition rate can be accurately obtained using two pressure sensors. Therefore, a vapor deposition film can be formed at an accurate vapor deposition rate, and a desired film thickness can be obtained. It is not necessary to replace the crystal unit, which was necessary when using the crystal unit type film thickness sensor, and the deposition rate can be continuously measured for a long time without returning the vacuum chamber to the atmosphere. Therefore, it is possible to perform continuous vapor deposition for a long time, and a decrease in productivity can be avoided. Since the pressure in the evaporation source can be measured by the first pressure sensor, the heating temperature in the evaporation source and the evaporation amount of the vapor deposition material based on the heating temperature can be accurately monitored and adjusted based on the pressure. it can.

Moreover, according to this invention, the vapor deposition rate of two vaporization materials can be separately measured correctly using four pressure sensors. Therefore, the vapor deposition film by each vapor deposition material can be formed with an exact ratio and vapor deposition rate, and a desired film thickness can be obtained. It is not necessary to replace the crystal unit, which was necessary when using the crystal unit type film thickness sensor, and the deposition rate can be continuously measured for a long time without returning the vacuum chamber to the atmosphere. Therefore, it is possible to perform continuous vapor deposition for a long time, and a decrease in productivity can be avoided.
Since the pressure in the first evaporation source and the second evaporation source can be measured by the first pressure sensor and the third pressure sensor, the heating temperature in the first evaporation source and the second evaporation source based on the pressure, and the The evaporation amount of the first vapor deposition material and the evaporation amount of the second vapor deposition material based on the heating temperature can be accurately monitored and adjusted.
By adjusting the pressure of the third pressure sensor and the fourth pressure sensor, it is possible to prevent the inflow of the first evaporating material into the second evaporation source and the back flow of the second evaporating material.

It is a block diagram of the vapor deposition apparatus which concerns on Embodiment 1 of this invention. It is a block diagram of the controller of the vapor deposition apparatus. It is a figure which shows the characteristic of the vapor deposition rate in the vapor deposition apparatus, and the pressure difference of two pressure sensors. It is a block diagram which shows the modification of the vapor deposition apparatus of FIG. It is a block diagram which shows another modification of the vapor deposition apparatus of FIG. It is a block diagram of the vapor deposition apparatus which concerns on Embodiment 2 of this invention. It is a block diagram which shows the modification of the vapor deposition apparatus of FIG.

  Hereinafter, embodiments of the present invention will be described with reference to the drawings.

[Embodiment 1]
FIG. 1 is a configuration diagram of a vapor deposition apparatus according to Embodiment 1 of the present invention.
As shown in FIG. 1, in a vacuum chamber 11 (deposition container), evaporating material (for example, on the surface (lower surface) of a glass substrate 12 (deposition target member) in a vacuum atmosphere of 1 × 10 ⁻³ Pa or less, for example. A vapor deposition chamber 13 (vacuum chamber) for depositing an organic EL material) is provided. The vacuum chamber 11 is formed with a vacuum port (not shown) that is evacuated by a vacuum unit. A work holder 15 for holding the glass substrate 12 is provided on the upper portion of the vacuum chamber 11. The vapor deposition apparatus of the present embodiment is an up-blow type (up deposition) vapor deposition apparatus that vaporizes an evaporation material from below on the lower surface (deposition surface) of the glass substrate 12 held by the work holder 15.

Outside the vacuum chamber 11, a material storage container 19 (crucible) is provided as an evaporation source for storing the vapor deposition material 16 and heating the vapor deposition material 16 by heating means such as a heater to obtain the evaporation material. The evaporated material obtained in the material storage container 19 is supplied to a material transport pipe 17 (guidance path) provided at the lower part of the vacuum chamber 11.
Outside the vacuum chamber 11, the flow rate control for controlling the flow rate of the evaporation material supplied from the material storage container 19 to the material transport pipe 17 by adjusting the opening degree between the material storage container 19 and the material transport pipe 17. A valve 18 is provided.

  Connected to the downstream end of the material transport pipe 17 is a discharge member 14 that discharges the evaporating material flowing from the material transport pipe 17 to the deposition target member by narrowing the flow path. The discharge member 14 has a dispersion container 14a (manifold) for diffusing the evaporation material, and a throttle opening (not shown) for discharging the evaporation material to the substrate 12 at the tip thereof. And a plurality of nozzle members 14b.

A first pressure sensor 21 that detects the pressure in the material storage container 19 is provided in the material storage container 19 upstream of the flow control valve 18. A second pressure sensor 22 that detects the pressure in the vapor deposition chamber 13 is provided in the vapor deposition chamber 13. For the pressure sensors 21 and 22, for example, heat conduction pressure sensors using heat conduction by gas molecules are used.
Since the pressure in the material storage container 19 can be measured by the first pressure sensor 21, the heating temperature in the material storage container 19 and the evaporation amount of the vapor deposition material 16 based on the heating temperature are accurately determined based on the pressure. Can be monitored and adjusted well.
From the viewpoint of the accuracy of the vapor deposition rate to be measured, the first pressure sensor is preferably installed at a location near the vapor deposition material 16 in the material storage container 19.

  Although not shown, in addition to the material container 19 (crucible), the material transport pipe 17, the discharge member 14, the flow rate control valve 18, and the pressure sensors 21 and 22 are configured by heating means such as a heater. Each component is heated to a temperature at which the evaporation material does not adhere. By making the temperature of the pressure sensors 21 and 22 higher than the ambient temperature by heating the pressure sensors 21 and 22, it is possible to avoid the evaporation material from adhering to the sensor portion, and continuous measurement is possible.

  By obtaining the flow rate Q of the evaporating material based on the difference (P1−P2) between the pressure P1 measured by the first pressure sensor 21 and the pressure P2 measured by the second pressure sensor 22, the glass substrate 12 of evaporating material is obtained. A controller 24 is provided for measuring the deposition rate R of the flow rate control valve 18 and controlling the opening degree of the flow rate control valve 18 so that the measured deposition rate R becomes a predetermined deposition rate Re.

Specifically, the pressure P1 measured by the first pressure sensor 21 and the pressure P2 measured by the second pressure sensor 22 are input to the controller 24, and the controller 24 sends a valve opening command L (valve to the flow control valve 18 to the flow control valve 18. An electrical signal corresponding to an opening degree of 0 to 100% is output.
As shown in FIG. 2, the controller 24 uses a first subtractor 31 that calculates a pressure difference between the input pressure P1 and the pressure P2 and a pressure difference (P1−P2) calculated by the first subtractor 31 as a material. A vapor deposition rate calculating unit 32 for obtaining a flow rate Q of the evaporating material flowing through the transport pipe 17 and obtaining a vapor deposition rate R of the evaporating material on the glass substrate 12 based on the obtained flow rate Q of the evaporating material; And a second subtractor 33 for obtaining a deviation between the vapor deposition rate R obtained by the vapor deposition rate calculator 32 and a PI control for outputting a valve opening degree command L so as to eliminate the deviation obtained by the second subtractor 33. The unit 34 is configured.

In the vapor deposition rate calculation unit 32, the material transport pipe is based on the difference (P1-P2) between the pressure P1 (Pa) measured by the first pressure sensor 21 and the pressure P2 (Pa) measured by the second pressure sensor 22. The flow rate Q (Pa · m ³ / sec) of the evaporation material is obtained by the following equation (1) using the synthetic conductance C (m ³ / sec) of each constituent member such as 17. Next, based on the fact that the vapor deposition rate R is proportional to the flow rate Q of the evaporation material, the vapor deposition rate R (Å / s) is obtained by the following equation (2) using the proportional multiplier F.
Q = C × (P1-P2) (1)
R = F × Q = G × (P1-P2) (2)
G = F × C
FIG. 3 shows an example of the relationship between the deposition rate R and the pressure difference (P1-P2).
Incidentally, combined conductance C of the components, the flow control valve 18, the material transport pipe 17, the dispersion container 14a, the conductance of the nozzle member 14b, as _{C 1,} C 2, _{C 3,} and _{C 4,} respectively, the following equation It is calculated by (3).
1 / C = 1 / C ₁ + 1 / C ₂ + 1 / C ₃ + 1 / C ₄ (3)

The above multiplier G is the type of the evaporation material, the heating temperature of the vapor deposition material 16 in the material storage container 19 (crucible), the shapes, dimensions, and materials of the material transport pipe 17 and the discharge member 14, and the nozzle member 14b and the glass substrate. 12 and can be obtained in advance by experiments. An example of a specific method for actually measuring the deposition rate R using the pressure sensors 21 and 22 will be described below.
a. A quartz-vibration film thickness sensor is provided beside the glass substrate 12, and vapor deposition is performed so that the indicated value X of the film thickness sensor becomes a substantially constant value.
The vapor deposition rate R at this time is obtained by the following equation (4), where Dv is the vapor deposition film thickness measured by the quartz vibration film thickness sensor and T is the vapor deposition time.
R = Dv / T (4)
b. The gain of the film thickness sensor is adjusted so that the indicated value X of the film thickness sensor becomes the same as the vapor deposition rate R obtained by the above formula, and the film thickness sensor value is calibrated.
c. The deposition rate R is changed, the pressures P1 and P2 are measured by the pressure sensors 21 and 22, and the relationship between the film thickness sensor instruction value X and the pressure difference (P1−P2) between these pressure sensors 21 and 22, that is, the multiplier G is obtained. Ask.
d. From the above relationship, the deposition rate R is measured based on the pressure difference (P1-P2).

  With the above configuration, the flow rate Q of the evaporation material discharged from the discharge member 14 is determined by determining the difference (P1−P2) between the pressure values measured by the first pressure sensor 21 and the second pressure sensor 22. The deposition rate R is continuously measured based on the fact that the flow rate Q of the evaporation material is proportional to the deposition rate on the glass substrate 12. A valve opening command L is output to the flow control valve 18 so that the measured deposition rate R becomes a predetermined deposition rate Re, and the opening of the flow control valve 18 is controlled according to the output signal. That is, the flow rate of the evaporation material supplied from the material storage container 19 to the material transport pipe 17 is controlled. Thereby, the flow rate Q of the evaporation material is controlled to a predetermined flow rate corresponding to the predetermined deposition rate Re, and the evaporation material is deposited on the glass substrate 12 at the predetermined deposition rate Re.

The vapor deposition method using the vapor deposition apparatus of Embodiment 1 is as follows.
Heating the vapor deposition material 16 in the material storage container 19 to obtain an evaporation material;
Transferring the evaporated material obtained in the material storage container 19 to the material transport pipe 17;
A step of discharging the evaporation material from the material transport pipe 17 to the glass substrate 2 through the discharge member 14;
Adjusting the flow rate of the evaporation material supplied from the evaporation source to the material transport pipe 17 using the flow rate control valve 18;
Detecting the pressure in the material container 19 using the first pressure sensor 21;
Detecting the pressure in the evaporation chamber 13 using the second pressure sensor 22;
Using the controller 24, the flow rate Q of the evaporation material is obtained based on the difference (P1-P2) between the pressure P1 measured by the first pressure sensor 21 and the pressure P2 measured by the second pressure sensor 22. The evaporation rate R of the evaporation material on the glass substrate 12 is measured based on the flow rate Q of the evaporated material, and the opening degree of the flow rate control valve 18 is adjusted so that the measured evaporation rate R becomes a predetermined evaporation rate Re. A controlling step;
including.

As described above, according to the first embodiment, the relationship between the pressure value difference (P1−P2) measured in advance by the two pressure sensors 21 and 22 and the vapor deposition rate R is used using the crystal oscillator type sensor. As a result, the deposition rate R can be measured only with the pressure sensors 21 and 22 without using the quartz vibrator type film thickness sensor. Compared to a conventional apparatus provided with one pressure sensor, the deposition rate R can be determined accurately, and as a result, the evaporation material can be deposited on the glass substrate 12 at an accurate predetermined deposition rate Re. . That is, a vapor deposition film can be formed at an accurate vapor deposition rate, and a desired film thickness can be obtained.
In addition, it is not necessary to replace the crystal unit that is necessary when the crystal unit type film thickness sensor is used, and the deposition rate R can be continuously measured without returning the vacuum chamber 11 to the atmosphere. Therefore, continuous vapor deposition for a long time is possible, and a decrease in productivity can be avoided.

  In the present embodiment, the first pressure sensor is installed in the material storage container 19. However, as shown in FIG. 4, a connection member such as a connection flange 20 is provided between the material storage container 19 and the flow rate control valve 18. In this case, the first pressure sensor 21 may be installed on the connection flange 20. By removing the material storage container 19 from the connection flange 20 when the vapor deposition material 16 is loaded into the material storage container 19, the vapor deposition material 16 does not touch the pressure sensor 21 when the vapor deposition material 16 is charged, and good measurement accuracy is maintained. can do. What is necessary is just to install the 1st pressure sensor 21 in the position which can detect the pressure in the material storage container 19. FIG.

  In the present embodiment, the pressure sensor 21 is provided as shown in FIG. 1, but as shown in FIG. 5, a space 25 other than the region where the vapor deposition material 16 is introduced is provided, and the pressure sensor 21 is installed in the space 25. It may be provided. The vapor deposition material 16 does not touch the pressure sensor 21 when the vapor deposition material 16 is charged, and good measurement accuracy can be maintained.

[Embodiment 2]
FIG. 6 is a configuration diagram of a vapor deposition apparatus according to Embodiment 2 of the present invention. Description of constituent members having the same reference numerals as those in FIG. 1 is omitted.
The vapor deposition apparatus according to the second embodiment simultaneously covers the first evaporation material (host material) and the second evaporation material (dopant material) having a smaller evaporation amount than the first evaporation material, that is, having a low concentration during evaporation. It has a configuration in which co-deposition can be performed to adhere to the vapor deposition member. The concentration ratio between the first evaporation material and the second evaporation material is, for example, 10 to 100: 1. Such a vapor deposition apparatus is used, for example, when two organic materials are simultaneously formed in order to improve luminous efficiency when an organic EL device is manufactured.

Outside the vacuum chamber 11, the first vapor deposition material 16A is accommodated, and the first vapor deposition material 16A is heated by a heating means such as a heater to obtain the first vaporization material. A crucible) is provided. The first evaporation material obtained in the first material storage container 19 </ b> A is supplied to a first material transport pipe 45 </ b> A (first induction path) provided in the lower part of the vacuum chamber 11.
Outside the vacuum chamber 11, the second vapor deposition material 16B is accommodated, and the second vapor deposition material 16B is heated by a heating means such as a heater to obtain a second vaporization material. A crucible) is provided. The second evaporation material obtained in the second material storage container 19B is supplied to a second material transport pipe 45B (second induction path) provided in the lower part of the vacuum chamber 11.

  The material transport tube 45 having the first material transport tube 45A and the second material transport tube 45B further joins the first material transport tube 45A and the second material transport tube 45A, so that the first evaporation material and the second evaporation material are combined. A third material transport pipe 45C (third guiding path) that transports the third evaporating material mixed with the material is provided.

  A discharge member 44 that discharges the third evaporating material flowing from the third material transport pipe 45C to the glass substrate 12 by narrowing the flow path is connected to the downstream end of the third material transport pipe 45C. The discharge member 44 is provided with a dispersion container 44 a for diffusing the third evaporation material and a throttle opening (not shown) for protruding the third evaporation material to the glass substrate 12. And a plurality of nozzle members 44b at the tip.

Outside the vacuum chamber 11, by adjusting the opening between the first material storage container 19A and the first material transport pipe 45A, the first material supplied from the first material storage container 19A to the first material transport pipe 45A is adjusted. A first flow rate control valve 18A for controlling the flow rate of one evaporating material is provided.
Outside the vacuum chamber 11, by adjusting the opening between the second material storage container 19B and the second material transport pipe 45B, the second material supplied from the second material storage container 19B to the second material transport pipe 45B is adjusted. A second flow rate control valve 18B for controlling the flow rate of the 2 evaporation material is provided.

A first pressure sensor 41 for detecting the pressure in the first material storage container 19A is provided in the first material storage container 19A upstream of the first flow rate control valve 18A. A second pressure sensor 42 that detects the pressure in the vapor deposition chamber 13 is provided in the vapor deposition chamber 13. A third pressure sensor 47 for detecting the pressure in the second material storage container 19B is provided in the second material storage container 19B upstream of the second flow rate control valve 18B. A fourth pressure sensor 46 that detects the pressure in the second material transport pipe 45B is provided in the second material transport pipe 45B on the downstream side of the second flow control valve 18B.
For the first pressure sensor 41, the second pressure sensor 42, the third pressure sensor 47, and the fourth pressure sensor 46, for example, a heat conduction type pressure sensor that uses heat conduction by gas molecules is used.
Since the pressure in the first material storage container 19A can be measured by the first pressure sensor 41, the heating temperature in the first material storage container 19A and the first vapor deposition material based on the heating temperature are based on the pressure. The evaporation amount of 16A can be accurately monitored and adjusted. Since the pressure in the second material storage container 19B can be measured by the third pressure sensor 47, the heating temperature in the second material storage container 19B and the second vapor deposition material based on the heating temperature are based on the pressure. The evaporation amount of 16B can be accurately monitored and adjusted.
From the viewpoint of the accuracy of the vapor deposition rate to be measured, the first pressure sensor is preferably installed at a location close to the first vapor deposition material 16A in the first material storage container 19A. The second pressure sensor is preferably installed at a location close to the second vapor deposition material 16B in the second material storage container 19B.

  Although not shown, in addition to the first material storage container 19A and the second material storage container 19B, the material transport pipe 45, the discharge member 44, the first flow control valve 18A, the second flow control valve 18B, the first pressure The constituent members of the sensor 41, the second pressure sensor 42, the third pressure sensor 47, and the fourth pressure sensor 46 are heated to a temperature that prevents the evaporation materials from adhering to the constituent members by heating means such as a heater. Yes. By heating the first pressure sensor 41, the second pressure sensor 42, the third pressure sensor 47, and the fourth pressure sensor 46, the first pressure sensor 41, the second pressure sensor 42, the third pressure sensor 47, and the fourth pressure By making the temperature of the sensor 46 higher than the ambient temperature, it is possible to prevent each evaporation material from adhering to each sensor part, and continuous measurement is possible.

Based on the difference (P1−P2) between the pressure P1 measured by the first pressure sensor 41 and the pressure P2 measured by the second pressure sensor 42, the controller 24 ′ performs the first evaporation discharged from the discharge member 44. The flow rate Q1 of the material is obtained. Based on the obtained flow rate Q1 of the first evaporation material, the first evaporation rate R1 of the first evaporation material onto the glass substrate 12 is measured. A valve opening command L1 (an electric signal corresponding to 0 to 100% of the valve opening) is output to the first flow rate control valve 18A so that the measured first deposition rate R1 becomes a predetermined deposition rate Re1, The opening degree of the first flow control valve 18A is controlled according to the output signal.
The controller 24 ′ is discharged from the discharge member 44 based on the difference (P 3 −P 4) between the pressure P 3 measured by the third pressure sensor 46 and the pressure P 4 measured by the fourth pressure sensor 47. A flow rate Q2 of the second evaporation material is obtained. Based on the obtained flow rate Q2 of the second evaporation material, the second deposition rate R2 of the second evaporation material onto the glass substrate 12 is measured. A valve opening command L2 (an electric signal corresponding to 0 to 100% of the valve opening) is output to the second flow rate control valve 18B so that the measured second evaporation rate R2 becomes a predetermined evaporation rate Re2. The opening degree of the second flow control valve 18B is controlled according to the output signal.

The first vapor deposition rate R1 is obtained by the same method as that for the vapor deposition rate R of the first embodiment.
The second deposition rate R2 is obtained by the following method.
Based on the difference (P3-P4) between the pressure P3 (Pa) measured by the third pressure sensor 47 and the pressure P4 (Pa) measured by the fourth pressure sensor 46, the conductance Cv ( m ³ / sec), the flow rate Q2 (Pa · m ³ / sec) of the second evaporation material is obtained by the following equation (1a). Next, based on the fact that the second vapor deposition rate R2 is proportional to the flow rate Q2 of the second evaporation material, the second vapor deposition rate R2 (Å / s) is obtained by the following equation (2a) using the proportional multiplier F.
Q2 = Cv × (P3-P4) (1a)
R = F * Q = G * (P3-P4) (2a)
G = F × Cv
The multiplier G is obtained in advance using the method described in the first embodiment.

  The pressure P3 and the pressure P4 are measured by the third pressure sensor 47 and the fourth pressure sensor 46, and the pressure P3 upstream from the second flow control valve 18B is set to be lower than the pressure P4 downstream from the second flow control valve 18B. By enlarging, the inflow of the first evaporation material and the backflow of the second evaporation material into the second material storage container 19B can be prevented.

The vapor deposition method using the vapor deposition apparatus of Embodiment 2 is as follows.
Heating the first vapor deposition material 16A in the first material storage container 19A to obtain a first evaporation material;
Heating the second vapor deposition material 16B in the second material storage container 19B to obtain a second evaporation material;
A step of transferring the first evaporation material obtained in the first material storage container 19A into the first material transport pipe 45A;
Transferring the second evaporation material obtained in the second material storage container 19B into the second material transport pipe 45B;
A step of joining the first material transport pipe 45A and the second material transport pipe 45B and transferring a third evaporation material in which the first evaporation material and the second evaporation material are mixed into the third material transport pipe 45C;
Discharging the third evaporating material from the third guide path to the deposition target member via the release member;
Adjusting the flow rate of the first evaporation material supplied from the first material storage container 19A to the first material transport pipe 45A using the first flow rate control valve 18A;
Adjusting the flow rate of the second evaporation material supplied from the second material storage container 19B to the second material transport pipe 45B using the second flow rate control valve 18B;
Detecting the pressure in the first material storage container 19A using the first pressure sensor 41;
Detecting the pressure in the evaporation chamber 13 using the second pressure sensor 42;
Detecting the pressure in the second material storage container 19B using the third pressure sensor 47;
Detecting the pressure in the second material transport pipe 45B using the fourth pressure sensor 46;
Using the controller 24 '
The flow rate Q1 of the first evaporation material is obtained based on the difference (P1-P2) between the pressure P1 measured by the first pressure sensor 41 and the pressure P2 measured by the second pressure sensor, and the obtained first evaporation is obtained. The first deposition rate R1 of the first evaporation material on the glass substrate 12 is measured based on the material flow rate Q1, and the first flow rate is set so that the measured first deposition rate R1 becomes the predetermined first deposition rate Re1. The second evaporation material is controlled based on the difference (P3−P4) between the pressure P3 measured by the third pressure sensor 47 and the pressure P4 measured by the fourth pressure sensor 46, which controls the opening degree of the control valve 18A. The second evaporation rate R2 of the second evaporation material to the glass substrate 12 is measured based on the obtained second evaporation material flow rate Q2, and the measured second evaporation rate R2 is a predetermined first value. The second deposition rate Re2 2 controlling the opening of the flow control valve 18B;
including.

As described above, by using the four pressure sensors 41, 42, 46, and 47, the deposition rates R1 and R2 of the two evaporation materials can be individually and accurately measured. Therefore, each evaporation material can be vapor-deposited on the glass substrate 12 at an accurate predetermined vapor deposition rate Re1, Re2. That is, a vapor deposition film made of each evaporation material can be formed at an accurate ratio and vapor deposition rate, and a desired film thickness can be obtained.
When the deposited film becomes thicker as in the prior art, it is not necessary to replace the crystal resonator of the crystal resonator type film thickness sensor. Therefore, it is possible to perform continuous co-evaporation for forming two kinds of organic materials at the same time for a long time, and it is possible to avoid a decrease in productivity.
When using a quartz oscillator type sensor for co-evaporation, the deposition rates R1 and R2 cannot be measured individually. However, by using the four pressure sensors 41, 42, 46, and 47, the deposition rates R1 and R2 can be determined. It can be measured individually.

  In the second embodiment, as in the first embodiment, when a connection member such as the connection flange 20 shown in FIG. 4 is provided between the material storage containers 19A and 19B and the flow rate control valves 18A and 18B, the connection member Pressure sensors 41 and 42 may be installed in the

  In the second embodiment, similarly to the first embodiment, a space such as the space 25 shown in FIG. 5 may be provided in the material storage containers 19A and 19B, and the pressure sensors 41 and 42 may be provided in the space 25. The vapor deposition material 16 does not touch the pressure sensor 21 when the vapor deposition material 16 is charged, and good measurement accuracy can be maintained.

  In the second embodiment, one type of second vapor deposition material is used, but a plurality of different types of second vapor deposition materials may be used. In this case, a plurality of second material storage containers 19B and second material transport pipes 45B are provided, and the second flow rate control valve 18B and the third pressure are respectively provided for the second material storage containers 19B and the second material transport pipes 45B. A sensor 47 and a fourth pressure sensor 46 may be provided to store the second vapor deposition material in each of the second material storage containers 19B.

  As a modification of the second embodiment, a case where two types of second vapor deposition materials (vapor deposition material 16B-1 and vapor deposition material 16B-2) are used will be described with reference to FIG. A description of the same parts as those in FIG. 6 is omitted.

Outside the vacuum chamber 11, a material storage container 19B-1 for storing the vapor deposition material 16B-1 and heating the vapor deposition material 16B-1 by a heating means such as a heater to obtain a 2-1 evaporation material is provided. Yes. The 2-1 evaporation material obtained in the material storage container 19 </ b> B- 1 is supplied to a material transport pipe 45 </ b> B- 1 provided at the lower part of the vacuum chamber 11.
Outside the vacuum chamber 11, a 2-2 material storage container 19B-2 for storing the evaporation material 16B-2 and heating the evaporation material 16B-2 by heating means such as a heater to obtain a 2-2 evaporation material. Is provided. The 2-2 evaporation material obtained in the material storage container 19B-2 is supplied to a material transport pipe 45B-2 provided in the lower part of the vacuum chamber 11.
The third material transport pipe 45C joins the first material transport pipe 45A, the material transport pipe 45B-1, and the material transport pipe 45B-2.

Outside the vacuum chamber 11, by adjusting the opening between the material storage container 19B-1 and the material transport pipe 45B-1, the first material supplied from the material storage container 19B-1 to the material transport pipe 45B-1 is adjusted. A flow rate control valve 18B-1 for controlling the flow rate of the 2-1 evaporation material is provided.
Outside the vacuum chamber 11, by adjusting the opening between the material storage container 19B-2 and the material transport pipe 45B-2, the first material supplied from the material storage container 19B-2 to the material transport pipe 45B-2. 2-2 A flow rate control valve 18B-2 for controlling the flow rate of the evaporation material is provided.

A third pressure sensor 47-1 for detecting the pressure in the material storage container 19B-1 is provided in the material storage container 19B-1. The material transport pipe 45B-1 is provided with a fourth pressure sensor 46-1 for detecting the pressure in the material transport pipe 45B-1.
A fifth pressure sensor 47-2 for detecting the pressure in the material storage container 19B-2 is provided in the material storage container 19B-2. A sixth pressure sensor 46-2 for detecting the pressure in the material transport pipe 45B-2 is provided in the material transport pipe 45B-2.

The flow rate of the 2-1 evaporation material based on the difference between the pressure P3-1 measured by the 3-1 pressure sensor 47-1 and the pressure P4-1 measured by the 4-1 pressure sensor 46-1. The flow rate control valve is measured so that the deposition rate R2-1 of the 2-1 evaporation material on the glass substrate 12 is measured and the measured deposition rate R2-1 becomes the predetermined deposition rate Re2-1. A valve opening command L2-1 is output to 18B-1, the opening of the flow control valve 18B-1 is controlled in accordance with the output signal, and
The flow rate of the 2-2 evaporation material based on the difference between the pressure P3-2 measured by the 3-2 pressure sensor 47-2 and the pressure P4-2 measured by the 4-2 pressure sensor 46-2. The flow rate control valve is measured so that the deposition rate R2-2 of the 2-2 evaporation material on the glass substrate 12 is measured and the measured deposition rate R2-2 becomes the predetermined deposition rate Re2-2. A controller 54 is provided that outputs a valve opening command L2-2 to 18B-2 and controls the opening of the flow control valve 18B-2 in accordance with the output signal.

As described above, by using the six pressure sensors 41, 42, 46-1, 46-2, 47-1, and 47-2, the evaporation rates R1, R2-1, and R2-2 of the three evaporation materials can be set. It can be accurately measured individually. Therefore, each evaporation material can be vapor-deposited on the glass substrate 12 at an accurate predetermined vapor deposition rate Re1, Re2-1, Re2-2. That is, a vapor deposition film made of each evaporation material can be formed at an accurate ratio and vapor deposition rate, and a desired film thickness can be obtained.
When the deposited film becomes thicker as in the prior art, it is not necessary to replace the crystal resonator of the crystal resonator type film thickness sensor. Therefore, it is possible to perform continuous co-evaporation for forming two kinds of organic materials at the same time for a long time, and it is possible to avoid a decrease in productivity.
When using a quartz oscillator type sensor for co-evaporation, the deposition rates R1, R2-1, and R2-2 cannot be measured individually, but the six pressure sensors 41, 42, 46-1, and 46-2. , 47-1, 47-2, the deposition rates R1, R2-1, R2-2 can be individually measured.

  In Embodiment 1-2, although it is set as the structure of the up blow type (up deposition) which vapor-deposits evaporation material from the lower surface (deposition surface) of the glass substrate 12 hold | maintained at the workpiece holder 15, direction of a vapor deposition direction It is also possible to adopt a configuration that does not select any one, that is, a side depot or down depot configuration.

DESCRIPTION OF SYMBOLS 11 Vacuum chamber 12 Glass substrate 13 Deposition chamber 14 Release | release member 15 Work holding | maintenance tool 16 Deposition material 16A 1st vapor deposition material 16B 2nd vapor deposition material 17,45 Material transport pipe 18 Flow control valve 18A 1st flow control valve 18B 2nd flow control Valve 19 Material storage container 19A First material storage container 19B Second material storage container 21 First pressure sensor 22 Second pressure sensor 24, 24 ', 54 Controller 45A First material transport pipe 45B Second material transport pipe 45C Third material Transport pipe 46 Fourth pressure sensor 47 Third pressure sensor 18B-1, 18B-2 Flow rate control valve 19B-1, 19B-2 Material storage container 45B-1, 45B-2 Material transport pipe 46-1 Fourth 4-1 pressure Sensor 46-2 4-2 pressure sensor 47-1 3-1 pressure sensor 47-2 3-2 pressure sensor

Claims (7)

A vapor deposition apparatus for attaching an evaporation material to a vapor deposition member in a vacuum chamber,
An evaporation source for storing the evaporation material and heating the evaporation material to obtain the evaporation material;
A guide path for transferring the evaporation material obtained in the evaporation source;
A discharge member that discharges the evaporating material flowing from the guide path to the deposition target member;
A flow rate control valve for adjusting the flow rate of the evaporation material supplied from the evaporation source to the induction path;
A first pressure sensor for detecting the pressure in the evaporation source;
A second pressure sensor for detecting the pressure in the vacuum chamber;
By measuring the flow rate of the evaporating material based on the difference between the value measured by the first pressure sensor and the value measured by the second pressure sensor, the evaporating rate of the evaporating material to the vapor deposition member is measured and measured. A controller for controlling the opening degree of the flow rate control valve so that the deposited deposition rate becomes a predetermined deposition rate;
A vapor deposition apparatus comprising: The release member is
A dispersion vessel for diffusing the evaporation material;
A plurality of nozzle members protruding toward the deposition target member and having a throttle opening at the tip for discharging the evaporation material to the deposition target member;
The vapor deposition apparatus according to claim 1, comprising: In a vacuum chamber, a vapor deposition apparatus for adhering a third vaporized material, which is a mixture of a first vaporized material and a second vaporized material having a smaller vapor deposition amount than the first vaporized material, to a vapor deposition member,
A first evaporation source containing the first evaporation material and heating the first evaporation material to obtain the first evaporation material;
A second evaporation source containing the second evaporation material and heating the second evaporation material to obtain the second evaporation material;
A first induction path for transferring the first evaporation material obtained in the first evaporation source;
A second induction path for transferring the second evaporation material obtained in the second evaporation source;
A third induction path for transferring the third evaporation material in which the first evaporation material and the second evaporation material are mixed by joining the first induction path and the second induction path;
A discharge member that discharges the third evaporation material flowing from the third guide path to the deposition target member;
A first flow rate control valve for adjusting a flow rate of the first evaporation material supplied from the first evaporation source to the first induction path;
A second flow rate control valve for adjusting a flow rate of the second evaporation material supplied from the second evaporation source to the second induction path;
A first pressure sensor for detecting the pressure in the first evaporation source;
A second pressure sensor for detecting the pressure in the vacuum chamber;
A third pressure sensor for detecting the pressure in the second evaporation source;
A fourth pressure sensor for detecting the pressure in the second guiding path;
The first deposition of the first evaporation material onto the vapor deposition member is obtained by determining the flow rate of the first evaporation material based on the difference between the value measured by the first pressure sensor and the value measured by the second pressure sensor. A rate is measured, the opening of the first flow rate control valve is controlled so that the measured first deposition rate becomes a predetermined first deposition rate, and the value measured by the third pressure sensor; By determining the flow rate of the second evaporation material based on the difference from the value measured by the pressure sensor, the second evaporation rate of the second evaporation material to the evaporation target member is measured, and the measured second evaporation rate is A controller for controlling the opening of the second flow rate control valve so as to achieve a predetermined second deposition rate;
A vapor deposition apparatus comprising: The release member is
A dispersion vessel for diffusing the third evaporation material;
A plurality of nozzle members protruding toward the vapor deposition member and having a throttle opening at the tip for releasing the third evaporation material to the vapor deposition member;
The vapor deposition apparatus according to claim 3, comprising: A plurality of second evaporation sources and second induction paths;
A second flow rate control valve, a third pressure sensor, and a fourth pressure sensor are provided for each second evaporation source and second induction path,
5. The vapor deposition apparatus according to claim 3, wherein the second vapor deposition materials stored in the respective second evaporation sources are different from each other. A vapor deposition method using the vapor deposition apparatus according to claim 1,
Heating the vapor deposition material in an evaporation source to obtain the evaporation material;
Transferring the evaporation material obtained in the evaporation source into the induction path;
Discharging the evaporation material from the guide path through the discharge member to the deposition target member;
Adjusting the flow rate of the evaporation material supplied from the evaporation source to the induction path using the flow rate control valve;
Detecting the pressure in the evaporation source using the first pressure sensor;
Detecting a pressure in the vacuum chamber using a second pressure sensor;
Using the controller, the flow rate of the evaporating material is obtained based on the difference between the value measured by the first pressure sensor and the value measured by the second pressure sensor, and the evaporating material is obtained based on the obtained flow rate of the evaporating material. Measuring a deposition rate on the deposition target member, and controlling the opening of the flow rate control valve so that the measured deposition rate becomes a predetermined deposition rate;
The vapor deposition method characterized by including. A vapor deposition method using the vapor deposition apparatus according to claim 3,
Heating the first vapor deposition material in the first evaporation source to obtain the first evaporation material;
Heating the second vapor deposition material in the second evaporation source to obtain the second evaporation material;
Transferring the first evaporation material obtained in the first evaporation source into the first induction path;
Transferring the second evaporation material obtained in the second evaporation source into the second induction path;
Transferring the third evaporating material in which the first evaporating material and the second evaporating material are mixed into the third guiding path by joining the first guiding path and the second guiding path;
Discharging the third evaporating material from the third guide path to the deposition target member via the release member;
Adjusting the flow rate of the first evaporation material supplied from the first evaporation source to the first induction path using the first flow rate control valve;
Adjusting the flow rate of the second evaporation material supplied from the second evaporation source to the second induction path using the second flow rate control valve;
Detecting the pressure in the first evaporation source using the first pressure sensor;
Detecting a pressure in the vacuum chamber using a second pressure sensor;
Detecting a pressure in the second evaporation source using a third pressure sensor;
Detecting a pressure in the second taxiway using a fourth pressure sensor;
Using the controller
A flow rate of the first evaporating material is obtained based on a difference between a value measured by the first pressure sensor and a value measured by the second pressure sensor, and the first evaporating material is obtained based on the obtained flow rate of the first evaporating material. The first deposition rate of the material to the deposition target member is measured, the opening of the first flow rate control valve is controlled such that the measured first deposition rate becomes a predetermined first deposition rate, and the third pressure The flow rate of the second evaporating material is obtained based on the difference between the value measured by the sensor and the value measured by the fourth pressure sensor, and the second evaporative material coating is obtained based on the obtained flow rate of the second evaporating material. Measuring a second deposition rate on the deposition member, and controlling the opening of the second flow rate control valve so that the measured second deposition rate becomes a predetermined second deposition rate;
The vapor deposition method characterized by including.

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