TWI655407B - Crystal oscillating film thickness meter - Google Patents

Abstract

Provides the setting of a pre-formed base film on the electrode film (5) on the vapor deposition surface side of the crystal oscillator (4), suppresses the increase of the equivalent series resistance of the crystal oscillator, and achieves excellent crystal oscillation with a long life. Film thickness gauge.

A crystal oscillating film thickness meter is a film under a vacuum evaporation device (D) in which a vapor deposition material evaporated from an evaporation source (2) is deposited on a surface of a substrate (3) in a vacuum tank (1). The crystal oscillation type film thickness meter (M) for thickness control is formed by depositing an organic material composed of an organic substance containing at least one or more carbon atoms, which is different from the aforementioned vapor deposition material, on the crystal oscillator (4). An organic material base film (6) is formed on the electrode film (5) on the front side by vapor deposition in advance. The organic material base film (6) is vapor-deposited with the aforementioned vapor-deposited material, and the thickness of the vapor-deposited material is thus reduced. Or measure the evaporation speed.

Description

Crystal Oscillating Film Thickness Meter

The present invention relates to a crystal oscillation-type film thickness meter for controlling film thickness in a vacuum evaporation device that forms a thin film on a substrate in a vacuum tank that maintains decompressed air.

In the vacuum evaporation device for forming a thin film on a substrate in the vacuum evaporation method, a film thickness meter is used in order to control the film thickness and the evaporation speed (film thickness ratio). Although there are various types of film thickness meters depending on the measurement method, the crystal vibrator method is widely used.

The crystal oscillation film thickness meter using the crystal vibrator method is used when the resonance of the crystal vibrator is changed due to the change of its mass. For example, the resonance (oscillation frequency) changes In the measurement, the film thickness and the film thickness ratio are measured, and this is fed back to the heating control device of the evaporation source, and the film thickness ratio of the vapor-deposited film on the substrate is controlled to be constant, and the film thickness is managed.

In addition, when measuring the thickness of a crystal vibrating film thickness meter in this way, if the thin film is vapor-deposited on the electrode film of the crystal vibrator to be thick, the resonance will become unstable, or the equivalent series resistance of the crystal vibrator ( (Crystal impedance) If the current rises, the current flowing through the crystal oscillator will decrease, and the phenomenon that resonance cannot be measured occurs. For this reason, when the thickness is so thick that the resonance cannot be measured, it is determined that the lifetime of the crystal oscillator is used, and the crystal oscillator is switched to a new crystal oscillator and used.

Historically, in order to extend the life of this crystal vibrator, according to Patent Document 1 (Japanese Patent Laid-Open Publication No. 2000-101387), in order to produce a thin film that is vapor-deposited to a thickness that does not easily cause cracking and peeling of this film, A soft metal film is formed in advance on the electrode film on the film-forming surface side, thereby reducing the internal stress of the film and preventing peeling and cracking of the film.

In addition, according to Patent Document 2 (Japanese Patent Laid-Open Publication No. 2007-24909), a film is formed by sputtering, and the film-forming material used in the film-forming process is formed in advance on the surface of the film-forming side of the crystal oscillator so that The crystal vibrator is in close contact with the film-forming material, so the peeling of the crystal vibrator and the film-forming material can be suppressed.

[Prior technical literature] [Patent Literature]

[Patent Document 1] Japanese Patent Publication No. 2000-101387

[Patent Document 2] Japanese Patent Publication No. 2007-24909

However, it is known from Patent Documents 1 and 2 that a method of forming a film on a crystal vibrator in advance is a method of preventing the isolation of the film-forming material, eliminating the instability of resonance, and extending the life of the crystal vibrator. Even if the film on the vibrator is not peeled off, the equivalent series resistance of the crystal vibrator will still increase, and the current flowing through the crystal vibrator will decrease, making it impossible to measure resonance, so the life of the crystal vibrator cannot be extended.

That is, even if evaporation of the vapor-deposited film can be prevented, and when an organic material with a small specific gravity in the vapor-deposited material is vapor-deposited, the organic material is continuously formed on the electrode so that the larger the thickness of the vapor-deposited film becomes, the larger the thickness of the vapor-deposited film becomes. The thickness shear vibration of the crystal vibrator cannot be followed, so even if the vibration itself is maintained, the thicker the film thickness of the vapor-deposited film is, the higher the equivalent series resistance is. Therefore, the problem that the oscillation frequency cannot be set cannot be fully solved. Crystal oscillation The life of the film thickness gauge is still short and cannot be extended.

In particular, the vapor deposition materials used in the manufacture of organic EL devices are organic materials with a small specific gravity. They have poor adhesion to the electrode film (such as Au, Ag) on the surface of the crystal oscillator, and cannot follow the thickness shear vibration of the crystal oscillator. Since this organic material is only multiplied on the electrode film, if the film thickness of the vapor-deposited film increases, the equivalent series resistance increases, so the lifetime of the crystal oscillator is short.

The present invention is to find and solve the above problems, and the object is to provide an excellent crystal oscillatory film thickness meter, which uses an organic material composed of an organic material containing at least one carbon atom different from the vapor deposition material. The electrode film on the vapor-deposited surface side of the crystal vibrator is vapor-deposited in advance to form a base film of an organic material, and an increase in the equivalent series resistance of the crystal vibrator is suppressed, thereby achieving a long life.

The gist of the present invention will be described with reference to the drawings.

A crystal oscillation type film thickness meter is a crystal oscillation type for a film thickness control under a vacuum evaporation device D in which a vapor deposition material evaporated from an evaporation source 2 is deposited on a surface of a substrate 3 in a vacuum tank 1 to form a thin film The film thickness meter M is characterized in that an organic material composed of an organic substance containing at least one or more carbon atoms, which is different from the aforementioned vapor deposition material, is borrowed from the electrode film 5 on the vapor deposition surface side of the crystal oscillator 4. An organic material base film 6 is formed by vapor deposition in advance as a coating, and the aforementioned vapor deposition material is vapor-deposited on the organic material base film 6 to measure the film thickness or vapor deposition rate of the vapor deposition material.

In addition, as for the crystal oscillatory film thickness meter according to item 1 of the scope of the patent application, the organic material forming the organic material base film 6 is the one used in the vapor deposition process of the vapor deposition film density ratio on the substrate 3 surface. The evaporation material is still large.

In addition, as for the crystal oscillation type film thickness meter according to the first patent application range, the electrode film 5 formed on the front surface and the back surface of the crystal oscillator 4 is formed of a plurality of metals including Al.

In addition, as for the crystal oscillation type film thickness meter according to the second patent application range, the electrode film 5 formed on the front surface and the back surface of the crystal oscillator 4 is formed of a plurality of metals including Al.

In addition, as for the crystal oscillatory film thickness meter according to any one of claims 1 to 4, the crystal oscillator 4 is set to have a curved surface on the surface or the back, and the end portion is larger than the central portion. Thin shape.

In addition, as for the crystal oscillation type film thickness meter as described in any one of claims 1 to 4, the method of vapor deposition on the surface of the substrate 3 The aforementioned vapor deposition material used is an organic material for manufacturing an organic EL device.

In addition, as for the crystal oscillation film thickness meter according to item 5 of the scope of patent application, the evaporation material used in the evaporation process to the surface of the substrate 3 is an organic material for manufacturing an organic EL device.

Since the present invention is constituted as described above, it is an electrode film made of an organic material composed of an organic substance containing at least one carbon atom different from the vapor deposition material and deposited on the vapor deposition surface side of the crystal vibrator by vapor deposition in advance. This is an excellent crystal oscillation type film thickness meter that forms an organic material base film to suppress the increase in the equivalent series resistance of the crystal oscillator and achieves a long life.

That is, an organic material base film is formed on an electrode film of a crystal vibrator in advance by depositing an organic material different from the vapor deposition process, so that the electrode film and the The adhesion of the organic material base film is good. In addition, the organic material base film is also in good adhesion with the aforementioned vapor deposition material. In addition, the compatibility with this vapor deposition material is also better than when the metal film is the base film. Compared with the metal film, the film interface is ambiguous. Even if the film thickness of the vapor-deposited film is increased, the increase in the equivalent series resistance of the crystal vibrator is still suppressed, so the life can be extended and it can be used for long-term monitoring. Crystal oscillation type film thickness meter for excellent film thickness control under vacuum deposition equipment.

In other words, the aforementioned organic material base film is formed on the electrode film of the crystal oscillator in advance, so that the adhesion between the electrode film and the evaporation material is poor, and the evaporation film is formed. The crystal oscillator cannot follow the resonance of the crystal oscillator, and when it is seen from the crystal oscillator, it is in a state where foreign matter is attached. Therefore, even in the case of vapor deposition of the energy loss for vibration and the equivalent series resistance of the crystal oscillator increases, The increase in the equivalent series resistance of the crystal vibrator at the time of evaporation is suppressed, so the life can be extended, and it becomes a crystal oscillation film thickness meter for film thickness control in an excellent vacuum evaporation device that can be monitored for a long time. .

In addition, as for the invention in the second scope of the patent application, the adhesion with the electrode film will be further improved, and it will become a more excellent crystal oscillation film thickness meter that can prevent peeling and cracking.

In addition, as for the inventions in the scope of patent applications Nos. 3 and 4, the adhesion between the system and the vapor deposition material will be further improved, which can prevent the vapor deposition film from following the resonance of the crystal vibrator and increase the equivalent series resistance of the crystal vibrator 4. As the current flowing through the crystal vibrator decreases, it becomes impossible to measure the resonance of a more excellent crystal oscillation film thickness meter after all.

In addition, as for the invention in the fifth scope of the patent application, the influence of the vibration of the end of the pressed crystal vibrator can be small, and the instability of resonance is suppressed, which becomes a more excellent one that can use the crystal vibrator for a longer time. Crystal Oscillating Film Thickness Gauge.

In addition, the inventions such as claims 6 and 7 of the scope of patent application are suitable for the manufacture of organic EL devices, and become more useful crystal oscillatory film thickness meters.

D‧‧‧Vacuum evaporation device

M‧‧‧ Crystal Oscillating Film Thickness Meter

1‧‧‧vacuum tank

2‧‧‧ evaporation source

3‧‧‧ substrate

4‧‧‧ crystal vibrator

5‧‧‧ electrode film

6‧‧‧ organic material base film

[Figure 1] Vacuum using the crystal oscillation film thickness meter related to this embodiment A schematic configuration diagram of a first example of a vapor deposition device.

[Fig. 2] A schematic configuration diagram of a second example of a vacuum evaporation device using the crystal oscillation film thickness meter according to this embodiment.

[Fig. 3] A schematic configuration explanatory diagram of the present embodiment.

[Fig. 4] A graph showing an equivalent series resistance value stabilization time ratio of the organic material vapor deposition to the film thickness of the organic material base film according to the embodiment.

Embodiments of the present invention which are considered to be suitable will be briefly explained by showing the effects of the present invention with reference to the drawings.

The crystal oscillating film thickness meter M of the present invention is used in the vacuum evaporation device D, and is used for controlling and managing the film thickness and the evaporation speed (film thickness ratio). The electrode film 5 on the side is previously vapor-deposited with an organic material made of an organic material containing at least one carbon atom to form an organic material base film 6, so that the vapor-deposited material is directly vapor-deposited on the electrode film 5. In the case, the adhesion between the electrode film 5 and the organic material base film 6 is good, and the adhesion between the organic material base film 6 and the aforementioned vapor deposition material is also good, and the compatibility with this vapor deposition material is also better than that of the metal film. The condition of the base film is still good, so the film interface is ambiguous compared to the metal film. Even if the film thickness of the vapor-deposited film of the evaporation material is increased, the increase in the equivalent series resistance of the crystal oscillator 4 is still suppressed, and the life can be extended. , Can be used for long-term monitoring.

For example, even when an organic material having a small specific gravity for manufacturing an organic EL device is vapor-deposited, the electrode film on the surface of a crystal vibrator (for example, For example, the adhesion of Au, Ag) is improved, and the followability of the thickness vibration of the crystal vibrator 4 is improved. The increase of the equivalent series resistance of the crystal vibrator 4 is suppressed, which can extend the life and can be monitored for a long time. .

Therefore, for example, an organic material that is vapor-deposited in advance to form an organic material base film 6 on the electrode film 5 is selected from those that are unlikely to increase the equivalent series resistance of the crystal vibrator during individual vapor deposition. For example, the choice is better than that of the organic material A as the vapor deposition material, and the electrode film 5 has a good adhesion, and the thickness of the crystal vibrator 4 has a higher follow-up of shear vibration. In addition, the compatibility with the organic material A also makes the metal film The condition of the base film is still good, making the film interface ambiguous. Even if the thickness of the vapor-deposited film is increased, the increase in equivalent series resistance can be suppressed, the oscillation frequency is stable and can be accurately measured, and the life can be increased. For this reason, the organic material B forming the organic material base film 6 is an organic material composed of an organic substance containing at least one carbon atom, which is different from the aforementioned vapor deposition material (organic material A).

In addition, when the base film is a metal film based on a metal material instead of the organic material B, even if the adhesion with the electrode film 5 is improved, a film interface with the vapor deposition material (organic material A) is generated. The effective series resistance increases and the life is short.

In addition, for example, if the film density is larger than that of the evaporation material deposited by the evaporation process, a dense film is formed, and the adhesion with the electrode film 5 is further improved. The mechanical strength of the film is higher than that of the evaporation process. The coating is further improved, which also prevents peeling and cracking.

For example, the organic material B forming the organic material base film 6 has a lower film density than the electrode film 5 but is larger than the vapor-deposited film, and adopts an intermediate film density. The mechanical strength of the film can also be improved.

Furthermore, the electrode film 5 formed on the front surface and the back surface of the crystal vibrator 4 is made of a plurality of metals containing Al, so that compared with the case where the electrode film 5 is formed of a metal having low reactivity such as Au and Ag, The adhesion to the vapor deposition material is good, the vapor deposition film cannot follow the resonance of the crystal vibrator 4, the equivalent series resistance of the crystal vibrator 4 rises, and the current flowing through the crystal vibrator 4 is reduced. In the end, the resonance cannot be measured. .

In addition, any one of the surface or the back surface of the crystal vibrator 4 is formed as a slightly convex curved surface, so that the impact of the vibration of the end of the pressed crystal vibrator 4 can be small, and the instability of resonance is suppressed, so that The crystal oscillator 4 can be used longer.

[Example]

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

This embodiment is a crystal oscillation type for controlling the film thickness in a vacuum evaporation device D in which the present invention is applied to a vacuum evaporation device D in which a vapor deposition material evaporated from an evaporation source 2 is deposited on the surface of a substrate 3 in a vacuum tank 1 Film thickness meter M.

FIG. 1 shows the schematic structure (first example) of the vacuum evaporation device D using the crystal oscillation film thickness meter M of this embodiment. However, in this embodiment, the internal structure of the vacuum tank 1 is as follows: An evaporation source 2 is disposed, a substrate holder 7 is disposed at a position opposite to the evaporation source 2, the substrate 3 is held by the substrate holder 7, and a vapor deposition material vaporized from the evaporation source 2 is deposited on the surface of the substrate 3 to form a thin film ( Evaporation film).

In this vacuum evaporation device D, a crystal oscillation type film thickness meter M is provided as a film thickness control monitor at a position that does not hinder the scattering process of the vapor deposition material emitted from the evaporation source 2 reaching the surface of the substrate 3 to form a thin film. , With a crystal vibrator 4.

The crystal oscillating film thickness meter M of this embodiment adopts the surface of the crystal vibrator 4 which is vibrated at a certain frequency by the transmitter 8, and the evaporation material emitted from the evaporation source 2 is stacked so that the resonance frequency is stacked. From the resonance frequency change, the evaporation rate and film thickness are calculated by the film thickness display section 11 and the value is fed back to the heating control section 9 to control the heater power of the evaporation source 2 to make the evaporation The plating speed becomes constant.

In addition, FIG. 2 illustrates a schematic configuration (second example) of a vacuum evaporation apparatus D that can be continuously used on a large substrate for a long time. The second example of the evaporation source 2 shown in FIG. 2 is a conventional point source, and a long-line source is arranged in a direction orthogonal to the substrate 3 or the transportation direction of the evaporation source 2 so that the large-sized substrate 3 can still be used. A uniform vapor deposition film is formed, and the amount of the vapor deposition material that can be accommodated in the evaporation source 2 becomes extremely large. Therefore, a long-term continuous vapor deposition becomes possible.

The crystal oscillating film thickness meter M, which is a film thickness control monitor in this embodiment, is provided with a plurality of crystal vibrators 4, and when the life of one crystal vibrator 4 comes, it is switched to another crystal vibrator 4 for use. , Making it possible to continuously monitor the evaporation speed over a longer period of time.

Furthermore, in order to prevent the amount of the evaporation material emitted from the evaporation source 2 from adhering to the surface of the crystal vibrator 4, a crystal vibrator 4 is used for a long period of time and is rotated at a constant speed. Non-open Interrupter 10 covering the mouth.

Thus, the crystal oscillation type film thickness meter M as the film thickness control monitor of this embodiment shown in the vacuum evaporation device D of FIG. 1 and FIG. 2 includes at least one or more different materials from the foregoing evaporation materials. An organic material made of an organic material of carbon atoms is formed on the electrode film 5 on the vapor deposition surface side of the crystal oscillator 4 by vapor deposition in advance to form an organic material base film 6.

In addition, the organic material that is vapor-deposited in advance to form the organic material base film 6 is selected as described above, and the equivalent series resistance of the crystal oscillator is unlikely to increase when it is vapor-deposited alone. Specifically, the selection is better than that of the organic material A as the evaporation material, and the electrode film 5 has a good adhesion, and the thickness of the crystal vibrator 4 has a higher follow-up shear vibration. In addition, the compatibility with the organic material A is also improved. The case where the metal film is a base film is still good, so that the film interface becomes ambiguous. Even if the thickness of the vapor-deposited film is increased, the increase of the equivalent series resistance can be suppressed, the oscillation frequency is stable and can be accurately measured, and the life can be increased. For this reason, as described above, the organic material B forming the organic material base film 6 is an organic material composed of an organic substance containing at least one carbon atom different from the vapor deposition material (organic material A) as described above.

In addition, in simple terms, when the base film is a metal film based on a metal material instead of the organic material B, even if the adhesion with the electrode film 5 is improved, an interface with the vapor deposition material (organic material A) is generated, which is equivalent. The series resistance increases and the life is short.

That is, the organic material B forming the organic material base film 6 is an organic material having good compatibility with the vapor deposition material (organic material A), and an organic material having higher adhesion than the organic material A and the electrode film 5 is used. A no The same organic material B.

In addition, in this embodiment, as described above, a film density higher than that of the vapor deposition material (organic material A) that is vapor-deposited in the vapor deposition process is used to increase the mechanical strength and prevent peeling and cracking.

In addition, the electrodes 5 formed on the front and back surfaces of the crystal vibrator 4 are made of an alloy mainly composed of Al, so that the electrode film 5 is formed of a metal having a lower reactivity than Au, Ag, or the like. In this case, the adhesion to the vapor-deposited material is improved, and an increase in the equivalent series resistance of the crystal oscillator 4 can be suppressed.

FIG. 3 is a schematic configuration of the crystal oscillator 4 of the present invention. As described above, an electrode film 5 made of an alloy containing Al as a main component is formed on the front and back surfaces of the crystal oscillator (crystal). Adopting Al system is easy to oxidize, and the surface of the electrode film 5 is formed with an oxide film covered with oxygen. The highly reactive oxygen molecules improve the adhesion between the organic molecules of the vapor-deposited organic material and the electrode film 5, and the vapor-deposited film will not It becomes impossible to follow the resonance of the crystal oscillator 4.

In addition, a slightly convex curved surface is taken on either the surface or the back surface that becomes the vapor deposition surface of the crystal vibrator 4, so that the vibration of the end of the pressed crystal vibrator 4 can be less affected, and the instability of resonance can be suppressed.

More preferably, the back side of the vapor-deposited surface of the crystal vibrator 4 is curved, so that the stability of the crystal vibrator 4 in the state where the material is attached during vapor deposition is improved.

Therefore, in this embodiment, an organic material base film 6 is previously formed on the electrode film 5 on the surface of the crystal vibrator 4 in advance, and the organic material B forming the organic material base film 6 is formed by crystal during separate evaporation. Zhen The equivalent series resistance of the mover 4 is not easily increased, and the organic material B has better adhesion to the electrode film 5 than the vapor deposition material (organic material A).

It is assumed that, as a preliminary film (base film) formed on the electrode film 5, when the metal film is vapor-deposited, the adhesion with the electrode surface is further improved. Since the interface of the organic material A used in the plating process is deteriorated, the problem cannot be solved.

Therefore, the use of organic material B in the organic material base film 6 (preparation film) not only improves the adhesion with the electrode film 5, but also is the same organic material as the organic material A used in the evaporation process. Good adaptability, film peeling is not easy to occur, and the film interface becomes ambiguous. Even if the film thickness increases, the increase in equivalent series resistance is still suppressed, which can prolong the life.

FIG. 4 shows an organic material base film 6 formed by vapor-depositing an organic material B on an electrode film 5 of a crystal vibrator 4 on a pre-evaporated preliminary film. The organic material base film 6 is vapor-deposited on the electrode film 5. In the case of the organic material A used in the program, the graph shows the time when the equivalent series resistance value does not rise and is stable.

The stabilization time of the equivalent series resistance value when the film thickness of the organic material base film 6 is 0.16 μm is 1, which represents the equivalent series resistance value of the organic material base film 6 when the film thickness is 0.78 μm, 1.57 μm, 3.13 μm. Settling time ratio.

When the film thickness of the organic material base film 6 is 0.16 μm, the film thickness of the organic material base film 6 becomes thicker to about 0.78 μm, 1.57 μm, or 3.13 μm, and the stabilization time ratio of the equivalent resistance value becomes longer. 1.3, 2.2, 6.8.

Therefore, the thicker the vapor-deposited organic material base film 6 is, the more effective it is to suppress an increase in the equivalent series resistance value.

In addition, the present invention is not limited to those in this embodiment, and the specific configuration of each constituent element can be appropriately designed.

Claims (7)

A crystal oscillating film thickness meter is a crystal oscillating film thickness meter for controlling film thickness under a vacuum evaporation device in which a vapor deposition material evaporated from an evaporation source is deposited on a substrate surface in a vacuum tank to form a thin film. The invention consists in that an organic material composed of an organic substance containing at least one or more carbon atoms, which is different from the aforementioned vapor deposition material, is formed on the electrode film on the vapor deposition surface side of the crystal vibrator by vapor deposition in advance to form an organic material. A material base film is formed by vapor-depositing the aforementioned vapor deposition material on the organic material base film, and measuring the film thickness or vapor deposition rate of the vapor deposition material. For example, the crystal oscillation film thickness meter of the first patent application range, wherein the organic material forming the organic material base film has a higher vapor deposition film density than the vapor deposition material used in the vapor deposition process on the substrate surface. . For example, the crystal oscillation type film thickness meter according to the first patent application range, wherein the electrode film formed on the front surface and the back surface of the crystal oscillator is formed of a plurality of metals including Al. For example, the crystal oscillation type film thickness meter according to the second patent application range, wherein the electrode film formed on the front surface and the back surface of the crystal oscillator is formed of a plurality of metals including Al. For example, the crystal oscillatory film thickness meter according to any one of the scope of application patents 1 to 4, wherein the crystal oscillator is set to have a convex curved surface or a back surface, and the end portion is thinner than the central portion. For example, the crystal oscillation type film thickness meter according to any one of claims 1 to 4, wherein the evaporation material used in the evaporation process to the substrate surface is an organic material for manufacturing an organic EL device. . For example, the crystal oscillation film thickness meter of the scope of application for patent No. 5, wherein the aforementioned vapor deposition material used in the vapor deposition process to the surface of the substrate is an organic material for manufacturing an organic EL device.