KR101814390B1 - Evaporation and sublimation method of vapor deposition materials in a vacuum vapor deposition apparatus, and crucible device for vacuum vaport deposition - Google Patents

Abstract

(assignment)
The present invention enables continuous operation over a long period of time while preventing deterioration of the evaporation material.
(Solution)
In the crucible holder 13, a radiant heat source 21 for radiating a heating wave whose infrared wavelength is the dominant wavelength is disposed in a heating wave transmission tube 22 made of a material which can transmit infrared rays. The heating waves from the radiant heat source 21 are irradiated to the surface of the evaporation material M in the crucible main body 12 and heated to evaporate or sublimate only the surface of the evaporation material M. Evaporated or sublimed evaporated material M is adhered to the surface of the heating wave transmission pipe 22 or the inner surface of the crucible main body 12 and the crucible holder 13, .

Description

TECHNICAL FIELD [0001] The present invention relates to a vapor deposition method, a sublimation method, and a vacuum deposition crucible for a vapor deposition material in a vacuum vapor deposition apparatus,

The present invention relates to a vapor deposition method and a vapor deposition method for a vapor deposition material which evaporates and sublimates by heating over a long period of time without deteriorating the vapor deposition material or the organic vapor deposition material in a vacuum vapor deposition apparatus, The present invention relates to a crucible device.

In a mass production process of a substrate (substrate) or the like for vacuum deposition, the vapor deposition material is heated for a long period of time, for example, for about one week to evaporate and sublimate, and the vapor deposition process is continuously performed. In such a long continuous operation, it is necessary to prevent the deterioration of the evaporation material by heating for a long time.

Conventionally,

A) A large number of crucibles containing a small amount of material consumed before deterioration of the evaporation material are prepared, and the crucible is successively replaced while sequentially operating.

B) Depositing the crucible while replenishing the material along with the reduction of the material.

C) The evaporation material formed in the form of a pellet is heated and locally heated by pressurizing the evaporation material to a heating member to evaporate or sublimate only the locality of the material, thereby preventing deterioration of the material at other portions, .

As a countermeasure for continuous operation for a long time, Patent Document 1 discloses a technique of heating an evaporation material to evaporate and sublimate the evaporation material in a state where a heating coil and an evaporation material are approaching by using an electric resistance type heating device in which a heating coil is disposed in a crucible Is proposed. In addition, other patent documents disclose that a vapor of evaporation material is evaporated and sublimated by a laser beam.

Japanese Unexamined Patent Application Publication No. 1-208452 (Fig. 1)

However, in the above A), there is a problem that a crucible replacing device is required in the evaporation chamber of a vacuum atmosphere, and the entire evaporation apparatus becomes large.

B), there has been a problem that the apparatus becomes complicated when a replenishing device for the evaporation material is required and the replenishment control is taken into consideration.

C), there is a problem that equipment for forming the evaporation material in the form of a pellet and a pressing device for pressing the evaporation material in the form of pellets to the heating source are required, which increases the equipment cost.

Further, in Patent Document 1, there is a problem in that when evaporated and sublimed evaporated materials are brought into contact with a heating device heated to a high temperature, they are thermally decomposed to lower the quality of the evaporated material, thereby adversely affecting film formation.

Further, in the conventional example of evaporating and sublimating the evaporation material by the laser beam, there is a problem that the evaporation material adheres to the inner surface of the crucible and is easily deposited.

An object of the present invention is to provide a vapor deposition, sublimation, and vacuum vapor deposition crucible for a vapor deposition material in a vacuum vapor deposition apparatus capable of continuous operation over a long period of time while preventing deterioration of the vapor deposition material by solving the above problems .

According to a first aspect of the present invention,

Evaporation and sublimation of an evaporation material in a vacuum evaporation apparatus in which an evaporation material (evaporation material) accommodated in a crucible is heated and evaporated or sublimated in a vacuum atmosphere to deposit the evaporation material on the surface of the evaporation material As a method,

A heating wave having a dominant wavelength of infrared rays is emitted from a radiant heater (radiant heater) arranged in the crucible through a heating wave transmitting container (heating wave transmitting container) at least a part of which is made of a material capable of transmitting infrared rays,

Only the surface of the evaporation material is heated and evaporated or sublimated by the heating wave,

Vaporizes, and sublimates the evaporated material attached to the inner surface of the crucible by the heating wave to evaporate or re-evaporate the evaporated material.

According to a second aspect of the invention, in the configuration of the first aspect,

The crucible is controlled to be lower than the evaporation temperature or the sublimation temperature of the evaporation material,

The refrigerant fluid is supplied into the heating wave permeation vessel to control the surface temperature to be less than the decomposition temperature of the evaporation material.

According to a third aspect of the present invention,

A crucible for vacuum vapor deposition which evaporates or sublimates an evaporation material accommodated in a crucible in a vacuum evaporation chamber (vacuum evaporation chamber) formed in a vacuum atmosphere to evaporate or sublimate the evaporation material on the surface of the evaporation material,

A radiating heat source (radiant heat source) for radiating a heating wave whose main wavelength is infrared (IR), and a heating wave permeable vessel at least partially made of a material which can transmit infrared rays and covering the radiant heat source, Placed,

The surface of the evaporation material is heated and evaporated or sublimated by the heating wave from the radiant heat source and the evaporation material sublimed or sublimated is heated by the heating wave to re-evaporate or re-sublimate the evaporation material adhered to the inner surface of the crucible To configure

The crucible is equipped with a vacuum evacuation feature.

According to a fourth aspect of the present invention, in the configuration of the third aspect,

A crucible temperature control unit for controlling the crucible to be below the evaporation temperature or below the sublimation temperature,

And a heater temperature control unit (heater temperature control unit) for supplying a coolant fluid into the heating wave permeation vessel to control the surface temperature of the heating wave transmission vessel and the decomposition temperature of the evaporation material.

According to a fifth aspect of the present invention, in the configuration according to the third or fourth aspect,

A plurality of said radiating heaters are arranged in said crucible,

A material concentration detector (material concentration detector) for detecting the concentration of evaporated or vaporized evaporated material is provided in the vacuum evaporation chamber,

And a film thickness control section for controlling the radiation heat so that the detection value of the material concentration detector becomes constant.

According to a sixth aspect of the present invention, in the configuration according to the third or fourth aspect,

A material concentration detector for detecting the concentration of evaporated or vaporized evaporated material is provided in the vacuum evaporation chamber,

A heat source position adjusting device (heat source position adjusting device) capable of moving in a direction approaching (away from) the surface of the evaporation material is provided in the heating wave permeation vessel,

And a film thickness control section for moving the radiation heat exchanger by the heat source position adjusting device so that the detection value of the material concentration detector becomes constant.

According to the invention as set forth in claim 1 or claim 3, since the heating wave is radiated from the radiant heat disposed in the crucible to heat only the surface of the evaporation material to evaporate or sublimate the evaporation material, So that the evaporation material in the crucible does not deteriorate even when continuous deposition is performed over a long period of time. Thus, the continuous deposition process can be performed for a long time with a simple structure. Further, even if the evaporated or sublimed evaporated material once adheres to the inner surface of the crucible, the heating wave from the radiant heat can be received and re-evaporated or re-sublimated. In addition, even if the evaporated or sublimed evaporated material once adheres to the surface of the heating wave permeable vessel, it can be re-evaporated or re-sublimated in a short time by receiving the heating wave from the radiant heat, .

According to the invention as set forth in claim 2 or 4, deterioration of the evaporation material in the crucible can be prevented by making the crucible less than the evaporation and sublimation temperature of the evaporation material. Further, since the refrigerant fluid is supplied into the heating wave permeation vessel to prevent the temperature rise of the radiant heat, the radiant heat can be stably operated. In addition, by making the surface temperature of the heating wave permeable vessel less than the decomposition temperature of the evaporation material, even if the evaporated or sublimed evaporated material is brought into contact with the surface of the heating wave permeable vessel, the film is not decomposed to adversely affect the film formation Do not.

According to the invention as set forth in claim 5, it is possible to control the irradiation amount of the heating wave radiated on the surface of the evaporation material easily by selectively operating a plurality of radiation heaters based on the detection value of the material concentration detector, The film thickness formed on the surface can be controlled with excellent precision.

According to the invention as set forth in claim 6, the radiant heat source is moved in the heating wave permeable container by the heat source position adjusting device to adjust the distance between the radiant heat source and the surface of the evaporation material, So that the film thickness formed on the surface of the evaporation material can be controlled with excellent precision.

Fig. 1 shows a vacuum deposition apparatus according to a first embodiment of the present invention, and is a configuration diagram of a up position type.
2 is an enlarged vertical sectional view of the crucible apparatus.
3 is a graph showing an example of discrimination of deterioration of an evaporation material.
4 is a longitudinal sectional view of a vacuum evaporation apparatus showing a modification A in which a crucible apparatus is provided in a vacuum evaporation chamber.
5 is a longitudinal sectional view showing a modification B of the vacuum deposition apparatus of the up position type.
Fig. 6 is a longitudinal sectional view showing a modified example C of radiant heat, in which an end closed type heating wave transmission pipe is provided. Fig.
7A and 7B are vertical cross-sectional views showing Modifications D1 and D2 in which the end-closed type heating wave penetrating tube is disposed through the bottom of the crucible. Fig. 7A is a cross- Type, and (b) is the radiant heat transfer type of the modification D2.
8 is an overall configuration diagram showing an example of a modification D2.
Figs. 9A to 9D show a modification E in which a plurality of radiant heaters are horizontally penetrated. Fig. 9A is a diagram showing a state in which a plurality of radiant heaters are installed at a predetermined pitch in the width direction, (C) is provided at a predetermined pitch in the width and height directions, and (d) is provided at a predetermined pitch in the height direction including the inside of the evaporation material.
10 is a configuration diagram showing an example of a modification E;
11 (a) to 11 (c) show a modification F in which a plurality of radiant heaters penetrate in a vertical direction, wherein (a) and (b) are longitudinal and transverse cross- (c) is a cross-sectional view in which three radiating heaters are arranged.
Figs. 12 (a) and 12 (b) are longitudinal and transverse cross-sectional views showing a cooling structure of a through-type heating wave penetration tube and showing a modification example G having a double pipe structure.
13 (a) to 13 (d) show the cooling structure of the end closed type heating wave transmission pipe, in which (a) and (b) (C) and (d) are a longitudinal sectional view and a transverse sectional view showing a modified example I of a double pipe structure in which a passage forming pipe is provided in a heating wave permeating pipe.
14 (a) and 14 (b) show the cooling structure of the crucible temperature control mechanism, wherein FIG. 14 (a) is a structural view showing a modified example J employing the forced cooling structure, Fig. 20 is a configuration diagram showing a modified example K adopted. Fig.

[Example]

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

[Example 1]

As shown in FIG. 1, this vacuum evaporation apparatus is configured as an up deposition type. The vacuum positioner of the up position type has a structure in which a substrate 1 which is a material to be evaporated through a support (not shown) is disposed on an upper portion of a vacuum evaporation chamber 2 formed by a vacuum container 1, (Substrate) 3 is disposed, and a material discharge port (material discharge port) 4 is disposed at the bottom. A material evaporator 11 for evaporating and sublimating the evaporation material M is provided outside the vacuum container 1. The material evaporator 11 is disposed outside the material outlet 4, Respectively. Although not shown in the drawing, the vacuum container 1 is provided with an opening (opening) to which a door for opening and closing the substrate 3 is attached.

2, the crucible provided in the material evaporator 11 includes a crucible body 12 having an upper surface opened to receive the evaporation material M, and a discharge port formed on the upper surface thereof. And a crucible holder 13 for housing the main body 12. [ Of course, the crucible body 12 may be formed as a single body or a single crucible holder 13.

The material evaporator 11 is provided with a radiant heater (radiant heater) 14 for radiating a heating wave having an infrared ray as a dominant wavelength, and the heater 11 for controlling the surface temperature of the radiant heater 14 A crucible temperature control section (16) for controlling the temperature of the evaporation material (M) through the crucible holder (13) and the crucible body (12), a control section (heater temperature control section) (Deposition control device) 18 provided with a film thickness control section 17 for controlling the thickness of the substrate 3 is provided.

(Radiant heat)

2, the radiation heat exchanger 14 includes a radiation heat source (radiation heat source) 21 for radiating a heating wave whose main wavelength is infrared, and a radiation heat source 21 for covering the radiation heat source 21, (Heating wave permeable vessel) 22 formed of a permeable material, and the heater temperature control unit 15 controls the temperature of the heating wave permeable tube 22 And a heater temperature control mechanism (heater temperature control mechanism) 20 for controlling the surface temperature to be less than the decomposition temperature of the evaporation material M is provided.

An infrared heater (lamp), a carbon heater (lamp), a halogen heater (lamp), or the like, which is made of a linear light source or a point light source, is used for the radiation heat source 21. Power for heating is supplied from the heating power source (heating power source) 29 to the radiating heat source 21 through a power source controller (power source controller)

The heating wave penetration pipe 22 is formed of a cylindrical vessel whose both ends are closed by an end member 22C. The crucible holder 13 and a refrigerant jacket 34 to be described later are provided with through holes which intersect at right angles with the respective central axes and which horizontally penetrate both side walls. And a pipe 22 is inserted and arranged. The heating wave transmission pipe 22 has a supporting portion 22A that is coupled to the through hole at both ends in the longitudinal direction and a supporting portion 22A which is in contact with the crucible holder 13 between these supporting portions 22A, (Transmissive portion) 22B made of a high-quality material such as a quartz tube or a glass-ceramics tube or the like. Of course, the whole of the heating wave transmission pipe 22 may be integrally formed of a material having a high infrared transmittance. A radiant heat source 21 is disposed in the transmission portion 22B of the heating wave transmission pipe 22 in correspondence with the central portion of the crucible holder 13.

Here, the quartz tube constituting the transmitting portion 22B has a very low absorption rate of infrared rays, so that it is considered that the heating wave transmission tube 22 is not heated by the heating wave. However, There is a possibility that the heating wave transmission tube 22 is heated up by heat conduction or heat accumulation from the heating wave transmission tube 22. The heater temperature control mechanism 20 is provided to solve this problem.

The heater temperature control mechanism 20 shown in Fig. 1 is for controlling the temperature of the heating wave transmission pipe 22 as described above. The heater temperature control mechanism 20 includes a heat exchanger 24A, a refrigerant tank 24B, A refrigerant pump 25 for supplying a refrigerant fluid (gas or liquid) into the heating wave transmission pipe 22, and a refrigerant pump 24 for supplying the refrigerant fluid (gas or liquid) And a heater temperature control unit 15 for controlling the refrigerant pump 25. The temperature of the coolant fluid is sent to the coolant tank 24B from the inside of the heating wave penetration pipe 22 to be detected by the temperature detector 24C and the cooler 24 is controlled by the heater temperature control unit 15 based on the detected temperature. So that the refrigerant fluid supplied into the heating wave transmission pipe 22 is controlled to a predetermined temperature. Accordingly, the surface temperature of the heating wave transmission pipe 22 can be made lower than the decomposition temperature of the evaporation material (M). Accordingly, even if the vaporized material M once evaporated / sublimated is brought into contact with the surface of the heating wave transmission tube 22, if the deposited evaporation material M is not decomposed and adversely affects the film formation There is no. Further, even if the evaporation material M adheres to the surface of the heating wave transmission tube 22 and solidifies, it can be re-evaporated / re-sublimated by the heating wave, and the transparency of the heating wave It is possible to prevent degradation.

In the first embodiment, the radiating heat source 21 is disposed directly in the heating wave transmission tube 22 so that the coolant fluid and the radiant heat source 21 are in direct contact with each other. However, in the radiant heat source 21, In the case of a halogen heater or the like, it is necessary to avoid direct contact of the refrigerant fluid. As a countermeasure to this, a space is formed on the same axial center in the heating wave transmission pipe 22 as shown in Modification G shown in Fig. 12, which will be described later, And a radiant heat source 21 is built in the protection inner pipe 46 so that the space portion between the heating wave transmission pipe 22 and the protection inner pipe 46 is filled with the refrigerant fluid It is good as a passage. Accordingly, even when the radiant heat source 21 is heated to a high temperature, the refrigerant does not directly come into contact with the radiant heat source 21, so that heating and temperature control can be performed more safely.

(Crucible)

The inner surface of the crucible main body 12 and the inner surface of the crucible holder 13 are each subjected to a mirror finish so that the reflectance of the heating wave is improved to prevent the surface temperature from rising due to heating waves.

The crucible temperature control mechanism 30 is for keeping the temperature of the evaporation material M of the crucible main body 12 below the evaporation / sublimation temperature. It is preferable that the lower limit temperature at this time be approximated to the evaporation / sublimation temperature to some extent in consideration of the performance of the radiation heat exchanger 14 and the running cost. For example, in the case of the organic EL material, There is a vaporizing material capable of appropriately vaporizing / sublimating the evaporation material M held by the heating wave only. Since the kind of the evaporation material M is very wide and the lower limit temperature can not be uniformly specified, Here, the lower limit temperature of the evaporation material (M) is set at room temperature.

The crucible temperature control mechanism 30 includes a crucible heating mechanism for heating the evaporation material M contained in the crucible main body 12, a crucible cooling mechanism for cooling the evaporation material M, And a crucible temperature control unit 16 for controlling the crucible temperature.

The crucible heating mechanism includes a heating coil 33 disposed on the outer circumferential surface and a bottom surface of the crucible holder 13 and a power controller 35 for supplying heating power to each heating coil 33 from the heating power source 29, And heats the evaporation material (M) contained in the crucible body (12).

The crucible cooling mechanism is a refrigerant circulation type and is provided with a refrigerant jacket 34 that covers the outer surface of the crucible holder 13 by the outer and bottom portions of the heating coil 33. The refrigerant jacket 34 is provided with, And cooling chambers 36a to 36c are vertically divided into three stages. A circulation type cooler (chiller) 37 for controlling evaporation, which has a heat exchanger 37A, a coolant tank 37B and a coolant fluid temperature detector 37C, and a cooler 37 for cooling the coolant from the cooler 37 And a crucible temperature control unit 16 for operating the cooler 37 and the coolant pump 38. The crucible temperature control unit 16 controls the temperature of the crucible 37,

In the above configuration, the temperature detector 37C detects the temperature of the refrigerant fluid discharged from the refrigerant tank 37B of the cooler 37 from the cooling chambers 36a to 36c, and the crucible temperature controller 16 detects the detected temperature The coolant is supplied to each of the cooling chambers 36a to 36c by operating the heat exchanger 37A and the coolant pump 38 of the cooler 37 to control the temperature of the coolant in the crucible main body 12 And the accommodated evaporation material (M) is cooled. Further, in the crucible heating mechanism, heating power is supplied from the power controller 35 to each heating coil 33 to heat the crucible holder 13. The evaporation material M contained in the crucible body 12 is controlled by the crucible temperature control unit 16 based on the detection value of the temperature detector 39 formed of a thermocouple provided in the crucible main body 12, , The evaporation temperature or the sublimation temperature, and is controlled to be in the range of room temperature or more. This is because, when the evaporation material M reaches or exceeds the evaporation temperature or sublimation temperature, evaporation or sublimation of the evaporation material M makes it difficult to control the amount of evaporation and deterioration of the evaporation material M is apt to be accelerated.

(Deposition material and decomposition temperature)

In the case of the organic EL material such as Alq3 as the evaporation material, since the evaporation temperature is 270 deg. C and the decomposition temperature is 430 deg. C, the evaporation temperature and the decomposition temperature are sufficiently separated. However, in the case of other organic EL materials, for example, there is an evaporation temperature approaching 200 deg. C and a decomposition temperature higher than 200 deg.

However, the evaporation / sublimation temperature referred to herein fluctuates more largely due to the pressure condition at the time of heating, and also greatly varies in the flow conditions (channel condition) and evaporation amount of the evaporation material discharged from the crucible. . In the case of the decomposition temperature, decomposition does not start suddenly at a predetermined temperature, but decomposition occurs in a part of the material even if the temperature is low. Here, the temperature at which the temperature rises and the decomposition rate of the material rapidly increases is defined as the decomposition temperature.

FIG. 3 is a graph showing the results of measurement of? -NDP by the PL measurement with respect to deterioration of the evaporation material M of the liquid crystal panel, and deterioration of the evaporation material M can be measured by PL measurement.

(Effect of Embodiment 1)

According to the first embodiment, heating waves are radiated from the radiant heater 14 disposed in the crucible holder 13 through the heating wave transmission tube 22 to heat only the surface of the evaporation material M to evaporate / sublimate The evaporation material M other than the surface is not exposed to a high temperature and the evaporation material M is not deteriorated even if evaporation / sublimation is performed by heating for a long time. Accordingly, a continuous deposition process for a long period of time can be performed with a simple structure.

The crucible body 12 and the crucible holder 13 can be controlled by the crucible temperature control mechanism 30 even if the evaporated / sublimed evaporated material M once adhered to the inner surface of the crucible main body 12 or the crucible holder 13 Deterioration of the deposited evaporation material M is prevented and the heating wave from the radiant heater 14 is received and adhered to the evaporation material M because the evaporation material 13 is controlled to be lower than the evaporation temperature or the sublimation temperature of the evaporation material M. [ The evaporated material M can be re-evaporated or re-sublimated.

Even if the vaporized / sublimed evaporated material M is brought into contact with the surface of the radiant heater 14, the heating medium temperature control mechanism 20 supplies the refrigerant fluid into the heating wave transmission tube 22, Since the surface is controlled at a temperature lower than the decomposition temperature, the evaporation material M is decomposed and does not adversely affect film formation. In addition, the radiant heat source 21 can be stably operated by the temperature control by the heater temperature control mechanism 20. Even if the vapor deposition material M adheres to the heating wave transmission tube 22 although the vaporized material M is hardly attached to the heating wave transmission tube 22, The permeability of the transmissive portion 22B of the heating wave transmission tube 22 is lowered and does not interfere with the irradiation of the heating wave.

The inner surfaces of the crucible main body 12 and the crucible holder 13 are mirror finished to improve the reflectivity of the heating wave so that heating of the crucible main body 12 and the crucible holder 13 by heating waves is suppressed, M can be prevented from deteriorating.

[Modification of Embodiment 1]

Modifications A to K of the first embodiment will be described with reference to Figs. 4 to 14. Fig. In Modifications A to K, the same components as those in the first embodiment are denoted by the same reference numerals, and a description thereof will be omitted.

Modifications A and B (arrangement of crucibles)

In the first embodiment, the material vaporizer 11 is provided outside the vacuum vapor deposition chamber 2. Alternatively, the material evaporator 11 may be provided inside the vacuum vapor deposition chamber 2 as shown in Modification A shown in Fig.

In the first embodiment, the upside position type in which the evaporation material M is adhered to the lower surface of the substrate 3 arranged in the horizontal posture from below is employed. However, as in the modification B shown in Fig. 5, Or a side deposition type in which the evaporation material M is adhered to the side surface of the substrate 3 from the side. Of course, the material evaporator 11 may be provided inside the vacuum evaporator chamber 2. According to Modifications A and B, the same operational effects as those of Embodiment 1 can be obtained.

Modifications C, D1, D2 (Radiative heat wave transmission tube and radiant heat source)

In the first embodiment, the tubular heat wave transmission tube 22 is of a horizontal and a horizontal type through which both sidewalls of the crucible holder 13 are respectively inserted and arranged in a horizontal posture. In the modification C shown in Fig. 6 And a tubular heating wave permeating tube 41 with its distal end closed is inserted from a through hole formed in one side wall of the crucible holder 13 to form a radiant heat source 41 at the tip of the heating wave transmitting tube 41 21) are disposed in the horizontal posture.

The modification D1 shown in Fig. 7 (a) is a modification example D1 shown in Fig. 7 (a), in which the heating wave transmission pipe 42 with the tip end closed is attached to the bottom of the crucible body 12 (crucible body 12 and / or crucible holder 13) And a radiant heat source 21 is fixedly disposed on the upper end of the heating wave transmission pipe 42. The heating radiation transmission pipe 42 is of a vertical one- According to these modified examples C and D1, the same operational effects as those of the first embodiment can be obtained. The cooling structure of these modified examples C and D1 is the same as the modified example H described later.

The modification D2 shown in Fig. 7 (b) and Fig. 8 is a modification example D2 in which the radiant heat source 21 is adjusted by the heat source position adjusting device 43 through the movable rod 44, It is possible. That is, the evaporation rate detector (material concentration detector) 5 provided in the vacuum evaporation chamber 2, the heat source position adjusting device 43 is operated by the film thickness control section 17 to move the movable rod 44 The distance between the surface of the evaporation material M and the radiation heat source 21 can be controlled. For example, when the evaporation amount of the evaporation material M is reduced, the movable rod 44 is retreated to lower the radiant heat source 21 so that the surfaces of the radiant heat source 21 and the evaporation material M approach each other, The evaporation amount of the material M can be increased. Thus, the evaporation material M can be uniformly evaporated and sublimated. Of course, it is possible to control the power supplied to the radiant heat source 21 by the power controller 28 to control the irradiation amount of the heating wave from the radiant heat source 21 in combination.

Variation E (plural radiating heat sources)

In the first embodiment, only one radiating heat exchanger 14 is disposed at a position above the evaporation material M, but as in the modification E shown in Figs. 9 (a) to 9 (d) A plurality of radiant heaters 14 may be provided at a predetermined interval in the example 1, the variant A) and the one through-hole type (variations B and C). The evaporation amount of the evaporation material (M) can be increased by the plurality of radiation heaters (14). In Fig. 9 (d), the lower radiant heater 14 is disposed through the evaporation material M, but these are used after the evaporation material M on the upper side is evaporated / sublimated.

10 is a view showing a configuration in which a lower radiant heater 14 is disposed in the evaporation material M as a modification E and a power controller (not shown) is connected to the film thickness controller 17 based on the detection value of the evaporation rate detector 5. [ The evaporation amount / sublimation amount of the evaporation material M can be effectively controlled by selectively operating the three radiation heaters 14 by operating the evaporator 28 and the refrigerant control valve 45. [ Of course, it is possible to control the power supplied to the radiant heat source 21 by the power controller 28 to control the irradiation amount of the heating wave from the radiant heat source 21 in combination.

Variation F (multiple radiant heat)

11 (a), 11 (b), and 11 (c), two or three radiation heaters 14 are arranged parallel to each other at a predetermined interval Can be installed. The evaporation amount of the evaporation material (M) can be increased by the plurality of radiation heaters (14). Of course, it is possible to control the power supplied to the radiant heat source 21 by the power controller 28 to control the irradiation amount of the heating wave from the radiant heat source 21 in combination.

Variation example G (cooling structure of radiant heat)

12 (a) and 12 (b) show a modification example G showing a cooling structure of the radial heat exchanger 14 of both lateral penetration type, and a refrigerant fluid channel is formed in the heating wave transmission tube 22, Is a double pipe structure in which a protective inner pipe 46 made of a material capable of efficiently transmitting infrared rays, for example, quartz, is disposed on the same axis and a radiant heat source 21 is embedded in the protective inner pipe 46, 21) is in direct contact with the refrigerant at a high temperature, there is a risk of being damaged.

Modification Example H (Radiative Heat Cooling Structure)

Figs. 13 (a) to 13 (c) show the cooling structure of the radiating heat exchanger 14 of one transverse penetration type. 13 (a) and 13 (b) show a modified example in which the inside of the heating wave transmission pipe 41 is partitioned by the boundary plate 47 and the refrigerant fluid supply path (supply path) 48A and the discharge path (discharge path) (48B). 13C and 13D show a modified example I in which a passage forming tube 49 is arranged in the heating wave permeating tube 41 and a space in the passage forming tube 49 and a space in the heating wave transmitting tube 41, And the passage forming tube 49 is used as the coolant fluid supply path 48A while the other is used as the discharge path 48B. The surface temperature of the heat wave transmission tube 41 of the transverse penetration type can be controlled with excellent precision by the respective cooling structures.

Similarly to Modification Example H, the cooling structure of the longitudinally penetrating type heating wave penetration pipe 42 can be divided into a heating wave transmission pipe and a boundary plate to form a supply path and a discharge path for the refrigerant fluid. In the same way as in Modification I, a passage forming tube is disposed in the heating wave permeating tube, and one of the space in the passage forming tube and the space between the heating wave transmitting tube and the passage forming tube is used as the refrigerant fluid supplying path, It can be made into an exhaust passage.

Modifications J, K (cooling structure of radiant heat)

Figs. 14 (a) and 14 (b) show a modification of the structure of the heater temperature control mechanism 20, which does not circulate when tap water or air is used as the refrigerant fluid. (a) shows a modification example J employing a forced circulation type cooling structure using a refrigerant pump 25, (b) shows a modification example K employing a natural circulation type cooling structure that does not use a refrigerant pump have.

M: Deposition material
1: Vacuum container
2: Vacuum deposition chamber
3: substrate (evaporation material)
5: Evaporation rate detector (material concentration detector)
11: Material evaporation device
12: Crucible body
13: Crucible holder
14: Radiant heat
15: heater temperature control section
16: crucible temperature control section
17:
18: Deposition control device
20: Heater temperature control mechanism
21: Radiant heat source
22: Heating wave permeation tube (heating wave permeation vessel)
22B:
24: Cooler
25: Refrigerant pump
28: Power controller
30: crucible temperature control mechanism
33: Heating coil
34: Refrigerant jacket
37: Cooler
38: Refrigerant pump
41: heating wave permeation pipe
42: heating wave permeation pipe
43: Heat source position adjusting device
44:
45: Refrigerant control valve
46: Inner protection
47: Boundary plate
49: passage forming tube

Claims (6)

Evaporation and sublimation of an evaporation material in a vacuum evaporation apparatus in which an evaporation material (evaporation material) accommodated in a crucible is heated and evaporated or sublimated in a vacuum atmosphere to deposit the evaporation material on the surface of the evaporation material As a method,
A heating wave having a dominant wavelength of infrared rays is radiated from a radiant heater (radiant heater) disposed in the crucible through a heating wave transmitting container (heating wave transmitting container) formed at least part of the infrared transmitting material,
Only the surface of the evaporation material is heated and evaporated or sublimated by the heating wave,
The crucible is controlled to be lower than the evaporation temperature or the sublimation temperature of the evaporation material,
Evaporates and sublimates and evaporates or re-evaporates the evaporation material attached to the inner surface of the crucible by the heating wave
And evaporating and evaporating the evaporation material in the vacuum evaporation apparatus.
The method according to claim 1,
A refrigerant fluid is supplied into the heating wave permeation vessel to control its surface temperature to be lower than the decomposition temperature of the evaporation material
And evaporating and evaporating the evaporation material in the vacuum evaporation apparatus.
A crucible for vacuum vapor deposition which evaporates or sublimates an evaporation material accommodated in a crucible in a vacuum evaporation chamber (vacuum evaporation chamber) formed in a vacuum atmosphere to evaporate or sublimate the evaporation material on the surface of the evaporation material,
A radiating heat source (radiant heat source) for radiating a heating wave whose main wavelength is infrared (IR), and a heating wave permeable vessel at least partially made of a material which can transmit infrared rays and covering the radiant heat source, Placed,
And a crucible temperature control unit for controlling the crucible to be below the evaporation temperature or below the sublimation temperature,
The surface of the evaporation material is heated and evaporated or sublimated by heating waves from the radiant heat source while controlling the crucible to a temperature lower than the evaporation temperature or sublimation temperature of the evaporation material, Is heated by the heating wave to re-evaporate or re-sublimate
The crucible is equipped with a vacuum evacuation feature.
The method of claim 3,
To the refrigerant fluid supply in the heat wave transmitted through the container, a heater temperature control part (加熱器溫度制御部) for controlling the surface temperature of the heat wave transmitted through the vessel to less than the decomposition temperature of the deposition material
Wherein the crucible is attached to the crucible.
The method according to claim 3 or 4,
A plurality of said radiating heaters are arranged in said crucible,
A material concentration detector (material concentration detector) for detecting the concentration of evaporated or vaporized evaporated material is provided in the vacuum evaporation chamber,
And a film thickness control section for controlling each of the radiation heaters so that the detection value of the material concentration detector becomes constant
The crucible is equipped with a vacuum evacuation feature.
The method according to claim 3 or 4,
A material concentration detector for detecting the concentration of evaporated or vaporized evaporated material is provided in the vacuum evaporation chamber,
A heat source position adjusting device (heat source position adjusting device) capable of moving in a direction approaching (away from) the surface of the evaporation material is provided in the heating wave permeation vessel,
It is preferable to provide a film thickness control section for moving the radiation heat exchanger by the heat source position adjusting device so that the detection value of the material concentration detector becomes constant
The crucible is equipped with a vacuum evacuation feature.

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