JPS5996263A - Vapor deposition device - Google Patents

Abstract

PURPOSE:To enable production of a film deposited by evaporation with good quality and the prevention of contamination in an electrode material and a space for vapor deposition by providing a gas discharge part consisting of a gas introducing pipe which leads a reactive gas to a specified position in a vapor deposition vessel and a discharging electrode provided around the circumference thereof in the vapor deposition vessel. CONSTITUTION:The inside of a bell-jar 30 is evacuated to a high degree of vacuum, via an evacuation path 38 having a butterfly valve 32, and a substrate 2 is heated with a heater 34. While the reactive gas activated or ionized by a gas discharge tube 37 connected to a gas introducing pipe 36 is introduced into the bell-jar, an evaporating source 25 is heated by the electron beam 27 from a heater 26 for an electron gun to evaporate a material to be deposited by evaporation, thereby forming a film deposited by evaporation on the substrate 2. The discharge part 37 is formed by winding an electrode 45 for electric discharge around gas introducing pipe 43, and enclosing the same with deposition preventive members 44, 46. The reactive gas is activated efficiently in the pipe 43 holding the high gaseous pressure without increasing the gaseous pressure in the space for vapor deposition. The electrode 45 is prevented from gaseous ion bombardment.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a vapor deposition apparatus configured to perform vapor deposition by introducing a reaction gas into a vapor deposition tank, and particularly to an apparatus called a reactive vapor deposition apparatus.

This type of reactive vapor deposition apparatus is, for example, an ITO (Indi
umTin Oxide) in the presence of ionized or activated oxygen gas.
The In-8n alloy and/or its oxides can be evaporated from the TO tablet and deposited onto the substrate.

D, C, ion blating, and RF ion brating devices are known as reactive vapor deposition devices. Among these, RF ion brating using high frequency discharge is disclosed in Japanese Patent Application Laid-Open No. 50-84474 and Japanese Patent Application Laid-Open No. 49-1989.
No. 113733 and Japanese Unexamined Patent Publication No. 49-120877. For example, as shown in FIG. 1, the substrate 2 is heated with a heater 34 in a vacuum chamber (Pelger) 30, and a predetermined voltage (-1
0V to -10kV) 35 is applied, while an AC voltage 71 is applied to the coil electrode 70 (high frequency discharge electrode) arranged on the evaporation source part.
The frequency of the alternating current is arbitrary, but high frequency (
For example, if 13.56 MHz) is used, the stability of discharge is good. ), the claw discharge generated between the substrate 2 and the electrode 70 activates or ionizes each atom of the unactivated reaction gas from the introduction tube 36 together with the vapor of the evaporated substance, for example, an ITO film is deposited on the substrate 2. to be deposited.

However, the above-mentioned known devices mainly have the following (1)
, (2) was found to have a fatal flaw.

(1), high frequency discharge is 10- to 10-'T or
Since it is carried out stably in a low vacuum of 10-
At a high degree of vacuum on the order of 5 to 1 O-4 Torr, the discharge becomes unstable and it becomes difficult to carry out reactive vapor deposition.

Therefore, in order to increase the adhesion strength of the deposited film and make the deposited film dense, it is necessary to apply a high voltage to the substrate to be deposited to accelerate the evaporated substance with an electric field. However, in the case of vapor deposition on an insulating substrate, for example, a glass or plastic substrate, it is difficult to provide a voltage applying means.

(2) Due to the large amount of evaporative substances adhering to the high-frequency discharge electrode, the adhering evaporative substances are bombarded and peeled off by discharge during long-term film formation, and this causes unstable discharge. It gets mixed into the evaporation source and makes the deposited film non-uniform.

Map ζ, evaporated substances adhere to the high frequency core input terminal, causing high frequency leakage.

The inventors of the present invention have discovered a device that can solve all of the above-mentioned problems by uniquely configuring the gas discharge section, and have arrived at the present invention.

A vapor deposition apparatus according to Pierchi, Inc., is configured to perform vapor deposition by introducing a reaction gas into a vapor deposition tank, in which the reaction gas is introduced from a gas inlet into a predetermined amount within the vapor deposition tank. The present invention is characterized in that a gas distribution section is provided within the vapor deposition facility, which comprises a gas introduction pipe leading to a location and a discharge electrode arranged around the gas supply pipe.

The vapor deposition apparatus according to the present invention has the following excellent features (1) to (3) as compared to the known apparatus described above.

(1) The discharge section is equipped with an inlet tube that guides the reaction gas from the gas inlet, and... The pressure can be maintained higher than the gas pressure in the space inside the deposition tank. Therefore, high-frequency discharge can be performed stably, and electric field acceleration of the evaporated substance is not required to lower the gas pressure in the space inside the deposition tank, making it possible to form a high-quality deposited film. .

(2) Since the discharge electrode is provided around the gas introduction tube, the gas in the introduction tube that maintains the gas pressure at a high level can be efficiently ionized or activated without increasing the gas pressure in the evaporation chamber. Therefore, ionized or activated gas components can be efficiently incorporated into the deposited film.

(3) Gas discharge occurs within the gas introduction tube, and the discharge electrode and high frequency introduction terminal are isolated from the discharge area, so bombardment by gas ions does not occur, and the material is heated, evaporated by bombardment, and manufactured. Contamination of the membrane space can be prevented.

DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described in detail below with reference to the drawings.

FIG. 2 shows a reactive vapor deposition apparatus according to this example. That is, 1℃
A butterfly valve 32 is attached to the Pelger 30 that forms an empty tank.
A vacuum pump (not shown) is connected through an exhaust path 38 having a vacuum pump, whereby the inside of the Pel jar 30 is brought into a high vacuum state of, for example, 10 -5 Torr to IF7 Torr. The substrate 2 is placed inside the Pelger 30 and heated by a heater 34 to a temperature of 600° C. or lower, preferably 300° C. or lower, and a gas discharge tube 37 (details will be described later) connected to the gas inlet 36 is heated. While introducing the activated or ionized reaction gas into the Pelger cabinet, the gas pressure was
), the evaporation material is heated and evaporated from the evaporation source 5 disposed in the pelger 30 so as to face the substrate 2. This heating means is an electron beam 27 by an electron gun heating device 2G.
Alternatively, a resistance heating method may be used. Further, a negative bias voltage 35 can be applied to the substrate 2 (actually, its back electrode (not shown)) as required.

What should be noted here is that the gas discharge tube 37 is constructed as shown in FIGS. 3 to 5.

That is, the discharge section 37 is detachably attached to the outwardly projecting tube section 30 a K provided on the Pel jar 30 via a plate 39 . For installation, a through hole (inlet) 40 is formed in the center of the plate 39 and is connected to the gas inlet 3G, and around this inlet 40 is a ring-shaped protrusion 41 with a small diameter.
and a large-diameter ring-shaped projection 42 are provided concentrically. A gas introduction pipe 43 is detachably fitted and fixed to the inner protrusion 41 so as to wrap around it, and a cylindrical anti-stick member 44 is similarly fitted and fixed to the outer protrusion 42. has been done.

For example, a coil-shaped discharge electrode 45 is wound between the outer periphery of the introduction pipe 3 and the inner periphery of the adhesion prevention member 44.

A common ring plate 46, which constitutes a part of the deposition prevention member, is fixed to the inner end surfaces of the introduction pipe 43 and the deposition prevention member 44 with screws 47, so that the introduction pipe 43 and the deposition prevention member 44 are connected to each other for discharge. It is attached to the plate 39 with the electrode 45 contained therein.

However, this attachment can be done in various ways or in various orders, and after the ring plate 46 is fixed as described above, the protrusion 41.4 is attached.
2 may be fitted at the same time.

For installation, a high frequency introduction terminal 48 connected to one end of an electrode 45 is fitted and fixed on the front plate of the plate 39, and a gas introduction pipe 50 from the outside is screwed into the center part through a threaded part 49. Fixed. Then, the plate 39 is fixed to the protruding tube portion 30a of the Pelger 30 by screwing the screws 52 into the screw holes 51 in the peripheral portion so as to close the opening 53. At this time, an O-ring 55 made of rubber, for example, for sealing is fitted into a ring-shaped groove 54 formed on the inner surface of the plate 39, and the protruding pipe portion 30a and the plate 39 are attached via this O-ring. Joined and fixed airtight.

As mentioned above, the gas discharge section 37 according to this example is attached to the plate 3.
It is removably attached within the Pelger 30 via the pin 9. Further, it is configured as an L-coupling type (inductively coupled type) using a coil electrode 45, and when a high frequency voltage is applied, ions or activation components of the reaction gas generated in the gas introduction tube 43 are released through the release opening 56. From there, it is led out to the internal space of Pelger 0 (that is, the flight space in which the evaporated substance portion flies toward the substrate 2).

To explain a specific example of the configuration of this reactive vapor deposition apparatus, in the trench discharge section 37, the gas introduction tube 43 is made of an insulating material, for example, an inner diameter of 2 to 10C7! It is made of Lφ quartz or Pyrex glass tube. The discharge electrode 45 is formed as a metal antenna wound around the introduction tube 43, and is, for example, a stainless steel pipe wound into a spiral circle with an inner diameter of 5 cIilφ to 20 cr/lφ (in this case, the pipe is filled with cooling water). (can be water-cooled from inside the entire electrode)
It consists of Further, the high frequency wave is introduced into the Jibel jar through the introduction terminal 48 after passing through a matching circuit (not shown) outside the Jibel jar. The other end of the electrode 45 is a free end. Anti-fouling member 44 (furthermore 4
6) covers the introduction tube 43 and electrode 45 to prevent evaporated substances from adhering to them and the high frequency introduction r6:a element 48, and prevents the high frequency power from drifting to stabilize the discharge. It is provided for the purpose of increasing the temperature and is necessarily made of a metal plate, such as stainless steel.

In addition, the above-mentioned introduction v50 is not a stainless steel or Teflon pipe, and the reaction gas (r
”: Oxygen, nitrogen, hydrogen, methane, depending on the type of steaming film.
A mixed gas of at least one of propane, silane, phosphine, diborane, arsine, etc. and an inert gas such as argon can be used.

The evaporated material IA (5 in Figure 2) is at least one selected from the group consisting of tungsten, molybdenum, chromium, iridium, tantalum, titanium, nickel, indium-tin, aluminum, silicon, its oxides, nitrides, etc. Examples include seeds. For example, in the film formation of ITOI, indium-tin and/or its oxide (η, human gas is oxygen +
Ar), silicon or aluminum and/or its nitride (introduced gas is N2) for forming a nitride film, and silicon (introduced gas is hydrogen) for forming an amorphous silicon hydride (a-8i:H) film. may be respectively applied as vaporized substances. For example, oxygen (flow rate 30 cc/min) using a mixed gas of oxygen and argon as the introduced gas.
, when introducing argon gas (flow rate 50 cc/ml), the degree of vacuum in the evaporation space inside the Pelger 30 is 10-5~
It is possible to maintain the pressure on the order of 10-4 Torr and to stably generate high-frequency discharge (introduced high-frequency power is OW to 3 KW) within the introduction pipe 43. Vacuum degree of vapor deposition space and introduction pipe 43
The relationship with the degree of vacuum inside can be arbitrarily adjusted by changing the flow rate of introduced gas, the flow rate of exhaust gas, the area of the gas discharge opening 56, etc. The area of the gas discharge opening 56 is, for example, 5 to 30
Preferably, it is c7Jt.

The reactive vapor deposition apparatus provided with the gas discharge section 37 as described above has the following features (1) to (5) compared to conventional apparatuses.

(1) By arranging the gas introduction pipe 43 close to the introduction port 36 (or 40), the gas pressure in the discharge region 57 can be maintained higher than the gas pressure in the vapor deposition space, resulting in stable High frequency discharge becomes possible.

Moreover, since the ions generated in the introduction tube 43 can be introduced into the Pelger immediately through the discharge opening 56, the amount of ions and the introduction efficiency can be increased. Furthermore, the gas pressure in the deposition space can be lowered, eliminating the need for electrical acceleration of the evaporated substance, allowing a wide selection of materials for the substrate to be deposited, and making it possible to form a high-quality deposited film.

(2) By arranging the discharge electrode 45 around the outer circumference of the introduction tube 43, the gas inside the introduction tube 43 can be efficiently ionized or activated by maintaining the gas pressure at a high level without increasing the gas pressure in the vapor deposition space. can be converted into In addition, since the force discharge region is limited within the discharge tube 43 and isolated from the electrode 45, the electrode 45 can be prevented from being bombarded by gas ions generated during discharge. In other words, it is possible to prevent the electrode material from being heated or evaporated by bombardment, thereby preventing contamination of the deposition space.

(3) Since the adhesion prevention members 44 and 46 were provided so as to enclose the introduction pipe 43 and the electrode 45, the introduction pipe 43, the electrode 45,
It is possible to prevent evaporated substances from adhering to the high-frequency introduction part 48, and also effectively prevent leakage of high-frequency waves through the mounting plate 39, electrode 45, and introduction pipe 43, so that discharge can be performed safely. be able to.

(4) This is different from the conventional structure of the discharge section, since the seal layer 55 is isolated from the gas discharge region 57 by the introduction pipe 43, etc. (it is not in contact with the discharge region 57).
Effect of discharge on seal member 55, for example seal Y1
．． 1j, gas IJ due to material damage and fatigue -Riku? It is possible to prevent deterioration of sealing properties such as

(5) Since the gas discharge part 37 can be easily attached to the wall of the Pelger 30 in some cases, it is easy to attach or remove it. Furthermore, since it is set in the protruding tube portion 30a that protrudes toward the evening of the vapor deposition space, it does not interfere with vapor deposition.

Although it is conceivable to configure the gas discharge section 37 as shown in FIG. 6, the intended purpose cannot be achieved with this. The discharge section 37 in FIG. 6 includes one cylindrical electrode member 62' having a gas inlet 61', and a cylindrical tube surrounding a discharge section l opening 163' with this one electrode member 62' provided at one end. It consists of a discharge space member 64' made of shaped glass, and another ring-shaped electrode part 66' having an outlet 65' provided at the other end of the discharge space member 64', and the one electrode member By applying a DC or AC voltage between 62' and the other electrode member 66', the gas inlet 61'
For example, hydrogen gas supplied through the discharge space 63' generates a glow discharge, whereby active hydrogen and ionized hydrogen ions consisting of hydrogen atoms or molecules activated by simulonic energy are released to the outlet 65'. It will be drained out. The discharge space member 64' in this illustrated example has a double pipe structure and is configured to allow cooling water to flow therethrough.
8' indicates the cooling water inlet and outlet. 69' is a cooling fin for one electrode member 62'. The distance between the electrodes in the hydrogen gas discharge tube 37 is 10 to 15 cTL,
The applied voltage is 600■, and the pressure in the discharge space 63' is 1O-2.
It is said to be about Torr. However, in this gas discharge section 37, the electrodes 62', 66', and the electrode mounting are connected to the discharge region 63' by sealing members (not shown), so they are exposed to gas ions generated during discharge. This results in the generation of contaminants, deterioration of sealing performance, etc., resulting in the discharging part not being able to withstand practical use.

In Figure 7, the discharge electrode is different from that in Figure 4, and the inlet tube lI.
A plurality of rings 45a arranged so as to enclose the circumferential surface of No. 3
, 45b. One of the ring-shaped electrodes 45a is connected to the high frequency introduction terminal 18 by a lead wire 67, and the other ring-shaped electrode 45b is connected to a metal anti-stick member 44 by a lead wire 58. The mounting is grounded via a plate 39. The electrodes 45a, 15b are, for example, made of copper or stainless steel and have an inner diameter of 2~]0cInφ and a width of 0.5~10cm7rL.
``From i-ring to C-coupling type (capacitive coupling type)
(The i:W ring can be cooled by wrapping a water-cooled tube around it.)

Next, an actual reactive vapor deposition apparatus using the above gas discharge section 37 will be explained with reference to FIGS. 8 and 9.

However, parts common to the above-described example are given common reference numerals, and their explanations may be omitted.

A gas discharge part 37 is attached to the vacuum (the same as described above for the Pelger 30 as a carbon dioxide) 2, while a sheet 2 as a substrate to be evaporated is placed facing the evaporator 15.
is sent from the supply roll 59 to the take-up roll 60. Adhesion prevention plates 61 and 62 are provided on both of these rolls, respectively. The substrate 2 is a heater (for example, a halogen lamp heater) with a reflector 65 arranged behind it through a wire mesh b3.
It is heated evenly by 3.1.

Full control of the thickness of the deposited film formed on the substrate 2.
- Film thickness meter (for example, a known crystal monitor) for checking 647%.

Such a deposition apparatus can be operated under the following conditions.

Evaporation material 252 TO tablets (Sn5 Jushano) Evaporation method: Electron gun heating/Deposition substrate 2: Metal sheet or resin (e.g. polyethylene terephthalate) sheet Cedar iris substrate 2 temperature near 0 to 300°C Introduced gas Dioxygen gas (30cc/min) and argon gas (50cc/min)
/min: to keep the amount of oxygen constant and adjust the degree of oxidation by oxygen). The flow rate can be controlled individually.

High frequency discharge device 37: The one shown in Fig. 3 or Fig. 7 (
(High frequency power: 50 W to 1 KW) That is, a mixed gas of oxygen and argon is ionized or activated by a discharge device 37, and while the ITO 25 is heated in an evaporation space 66 in the Pel jar 30, it is evaporated by heating with an electron gun. It was reacted with introduced gas ions or active gas components to be vapor deposited on the substrate 2. As a result, the evaporation rate of the evaporation material was set at 100 to 2000 A/min, and the conveyance speed of the substrate was set at 50 A/min.
~200cr/L/l1lin, the sheet resistance on the substrate is 500Ω/d~IMΩ/d, and the light transmittance is 8
It was possible to form an ITO film with a ratio of 0 to 90.

Although the present invention has been illustrated above, the above-mentioned example can be further modified based on the technical idea of the present invention.

For example, a plurality of the gas introduction pipes 43 described above can be provided, and as shown in FIG. 10, three introduction pipes 43 are arranged side by side,
Introductory tubes 50 are connected to each, and a common strip electrode 4 is connected to each other.
5a and 45b may be wrapped and attached.

This is advantageous because the ionized or activated gas components can be uniformly distributed over the deposition surface of the substrate 2. Further, the gas distribution can be arbitrarily adjusted depending on the arrangement of the gas introduction pipe. The number of discharge electrodes may be two or more, and the shape of the discharge electrodes, including the gas core inlet tube, may be rectangular or the like other than circular. Furthermore, the position and structure of the mounting location of the gas discharge section to the Pelger can be modified in various ways. Furthermore, the gas discharge portion may protrude into the deposition space of the Pelger.

Desirable results can also be obtained by arranging the gas discharge opening of the discharge section so as to face the substrate to be evaporated, or by arranging it so that the gas can be supplied near the substrate to be evaporated or the evaporation source.

[Brief explanation of the drawing]

FIG. 1 is a schematic cross-sectional view of a conventional RF ion blating device. Fig. 2 to Fig. 10 show examples of the present invention, in which Fig. 2 is a schematic sectional view of a reactive vapor deposition apparatus, Fig. 3 is an enlarged sectional view of a gas discharge section, and Fig. 4 is a gas discharge part. Figure 5 is a perspective view of the gas discharge section (however, the high-frequency discharge electrode is not shown)
6 is a cross-sectional view of a gas discharge section with a configuration different from that of the present invention, FIG. 7 is a perspective view of another gas discharge section, and Figure S8 is a schematic cross-sectional view of an actual reactive vapor deposition apparatus. , FIG. 9 is a sectional view taken along the line X--X in FIG. 7, and FIG. 10 is a perspective view of still another gas discharge section. In addition, in the reference numerals shown in the drawings, 2...... Vapor deposition target substrate 25... Evaporation material 26... Electron gun 30... ...Pelger 30a...Protruding pipe portion 34...H-p- 36,40...Gas fathom population 37... ...Gas discharge part 39...Mounted on plate 41.42...Protrusion, 13...Gas introduction pipe 44.46.61.62 ... Adhesion prevention member or adhesion prevention plate 45.45a, 45b ...Discharge electrode 48.
......High frequency introduction terminal 55...
・Sealing member 56...Gas release opening 57...Discharge area 59...Supply o-le 60... ...-8 Tori o - Le 64...
. . . Film thickness gauge 65 . . . Reflector plate 66 . . . Vapor deposition space. Agent Patent Attorney Hiroshi Aisaka (and 1 other person) No. 91■

Claims (1)

[Claims] 1. In a vapor deposition apparatus configured to perform vapor deposition by introducing a reaction gas into a vapor deposition tank, the reaction gas is introduced from a gas inlet to a predetermined location within the vapor deposition tank. 1. A vapor deposition apparatus, characterized in that a gas discharge section consisting of a gas introduction tube and a discharge electrode arranged around the gas introduction tube is provided in the vapor deposition tank. 2. A seal part for airtightly attaching the gas discharge part to the vapor deposition tank is provided at a position isolated from the discharge area of the gas discharge part. Apparatus according to claim 1. 3. According to claim 1 or 2, the gas introduction tube and the discharge electrode of the gas discharge section are provided with an anti-adhesion member for preventing evaporated substances from adhering thereto. 4. Apparatus according to any one of claims 1 to 3, in which the gas inlet tube comprises an insulating member. 5. The apparatus according to any one of claims 1 to 4, wherein a plurality of gas introduction pipes are provided, and a reaction gas is introduced into each of these pipes. 6. The device according to any one of claims 1 to 5, wherein at least one discharge electrode is arranged. 7. The device according to any one of claims 1 to 6, wherein the discharge electrode consists of a metal desk antenna wound around a gas introduction tube. 8. Any one of claims 1 to 6, wherein the tray for discharging consists of a plurality of ring-shaped metal electrodes arranged so as to enclose the circumferential surface of the gas introduction pipe. The device described in. 9. The device according to any one of claims 1 to 8, wherein the gas discharge section is detachably attached to the wall of the vapor deposition tank. 10. The apparatus according to claim 9, wherein the gas discharge section is removably attached to the vapor deposition tank via a plate. 11. For installation, a gas inlet is provided on the plate, and the gas inlet pipe is fixed so as to surround the 6 gas units [1].
''fA device according to claim 10. 12. Gasshi! 12. The device according to claim 11, wherein the L entry tube is removably fitted into a projection provided on the mounting plate. 1:3. The adhesion prevention member for preventing evaporated substances from adhering to the gas introduction pipe and the electric discharge plate is removably fitted and fixed to a protrusion provided on the plate. The apparatus described in any one of Items 10 to 12. 14. The apparatus according to any one of claims 10 to 13, wherein the peripheral part of the plate and the wall of the vapor deposition tank are fixed to each other via a sealing member. 15. An outwardly protruding tube portion that communicates with the inside and outside of the vapor deposition tank is provided, and a gas discharge section is disposed within this protruding tube section, and the opening of the protruding tube section is attached to a plate. 15. A device as claimed in claim 14, wherein the device is closed by.