JP2011181689A - Annealing device, annealing method and thin film substrate manufacturing system - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an annealing device which can heat a thin film formed on a surface of a substrate to higher temperature between the substrate and the thin film, and to provide an annealing method, and a thin film substrate manufacturing system. <P>SOLUTION: The annealing device 1 that anneals the thin film H formed on the surface of the substrate K by heating the substrate K and the thin film H by irradiating them with an electromagnetic wave includes: a calculating means of calculating the frequency of the electromagnetic wave irradiating the substrate K and the thin film H from a film thickness and resistivity of the thin film H; and an electromagnetic wave supply means of irradiating the substrate K and the thin film H with the electromagnetic wave having the frequency calculated by the calculating means. <P>COPYRIGHT: (C)2011,JPO&INPIT

Description

  The present invention relates to an annealing apparatus, an annealing method, and a thin film substrate manufacturing system for annealing a thin film on a substrate surface.

  After the thin film is formed on the substrate, the thin film is annealed to improve film characteristics such as electrical conductivity. For example, Patent Document 1 discloses an annealing apparatus that can efficiently cool a light emitting element without degrading maintainability.

JP 2009-295953 A

  By the way, depending on the substrate material, the glass transition point of the substrate may be lower than the annealing temperature of the thin film. In such a case, the substrate may be deformed and the thin film may be peeled off from the substrate. Therefore, the substrate material is limited to those having a glass transition point higher than the annealing temperature of the thin film.

  The present invention has been made in view of such circumstances, and an object of the present invention is to provide an annealing apparatus and an annealing apparatus capable of heating the thin film to a higher temperature among the thin film formed on the substrate and the substrate surface. A method and a thin film substrate manufacturing system are provided.

  In the annealing apparatus according to the present application, the substrate and the thin film formed on the surface of the substrate are irradiated with electromagnetic waves and heated, and in the annealing apparatus for annealing the thin film, based on the film thickness and resistivity of the given thin film, It is characterized by comprising calculation means for calculating the frequency of the electromagnetic wave applied to the substrate and the thin film, and electromagnetic wave supply means for applying the electromagnetic wave having the frequency calculated by the calculation means to the substrate and the thin film.

  The annealing apparatus according to the present application is characterized in that the calculation means calculates the frequency of the electromagnetic wave so that the penetration depth of the electromagnetic wave into the thin film corresponds to the film thickness of the thin film.

  The annealing apparatus according to the present application is characterized in that the electromagnetic wave supply means heats the thin film to a higher temperature than the substrate.

  An annealing apparatus according to the present application includes a cooling means for cooling the substrate.

  In the annealing method according to the present application, in the annealing method in which the substrate and the thin film formed on the substrate surface are irradiated with electromagnetic waves and heated, and the thin film is annealed, the substrate and the thin film formed on the basis of the thickness and resistivity of the thin film The frequency of the electromagnetic wave irradiated to the thin film is calculated, and the thin film is heated to a higher temperature than the substrate using the electromagnetic wave having the calculated frequency.

  The annealing method according to the present application is characterized in that the substrate is made of an organic material.

  An annealing method according to the present application is characterized in that the substrate is cooled.

  A thin film substrate manufacturing system according to the present application is provided with a film forming apparatus for forming a thin film on the surface of a substrate in a process of unwinding a flexible substrate wound around an unwinding roll and winding it on a winding roll. The thin film substrate manufacturing system includes the above-described annealing apparatus that anneals the thin film formed by the film forming apparatus under an arbitrary annealing condition, and the physical property measuring apparatus that measures the physical properties of the thin film annealed by the annealing apparatus. And

  The thin film substrate manufacturing system according to the present application includes a control device that receives a signal from the physical property measuring device and controls the operation of the film forming device, and the film forming device, the annealing device, and the physical property measuring device include the unwinding roll. And the physical property measuring device includes a transmission unit that transmits a predetermined signal to the control device, and the control device includes a transmission unit of the physical property measurement device. It has a means for stopping the operation of the film forming apparatus when the transmitted predetermined signal is received.

  In the thin film substrate manufacturing system according to the present application, the control device sets an annealing condition of the annealing device, and when the predetermined signal transmitted by the transmission unit of the physical property measuring device is received, the annealing device Means for changing the annealing conditions.

  The thin film substrate manufacturing system according to the present application includes substrate transfer means for unwinding and transferring the substrate from an unwinding roll at an arbitrary transfer speed, and winding the thin film substrate having a thin film formed on the substrate surface on a winding roll. And the control device controls the transfer speed of the substrate transfer means, and changes the transfer speed of the substrate transfer means when receiving the predetermined signal transmitted by the transmission means of the physical property measuring apparatus. It has the means to do.

  In the annealing apparatus according to the present application, the calculating means calculates the frequency of the electromagnetic wave applied to the substrate and the thin film formed on the surface of the substrate based on the thickness of the thin film and the resistivity of the thin film. The electromagnetic wave supply means irradiates the substrate and the thin film with electromagnetic waves having the calculated frequency.

  In the annealing apparatus according to the present application, the calculation means is based on the film thickness of the thin film and the resistivity of the thin film so that the penetration depth of the electromagnetic wave with respect to the thin film formed on the substrate surface corresponds to the film thickness of the thin film. Calculate the frequency of the electromagnetic wave.

  In the annealing apparatus according to the present application, the electromagnetic wave supply means irradiates the substrate and the thin film with electromagnetic waves having the calculated frequency, and heats the thin film to a higher temperature than the substrate.

  In the annealing apparatus according to the present application, the cooling means cools the substrate.

  In the annealing method according to the present application, the frequency of the electromagnetic wave applied to the substrate and the thin film is calculated based on the thickness and resistivity of the thin film formed on the substrate surface. The substrate and the thin film are irradiated with an electromagnetic wave having the calculated frequency, and the thin film is heated to a higher temperature than the substrate.

  In the annealing method according to the present application, the substrate irradiated with electromagnetic waves is made of an organic material.

  In the annealing method according to the present application, the substrate and the thin film are irradiated with electromagnetic waves while the substrate is cooled.

  The thin film substrate manufacturing system according to the present application includes a film forming apparatus, an annealing apparatus, and a physical property measuring apparatus. The film forming apparatus forms a thin film on a flexible substrate surface. The annealing apparatus is the above-described annealing apparatus that anneals the thin film formed by the film forming apparatus under an arbitrary annealing condition. The physical property measuring device measures the physical properties of the thin film annealed by the annealing device.

  The thin film substrate manufacturing system according to the present application includes a control device that receives a signal from the physical property measuring apparatus and controls the operation of the film forming apparatus. The film forming apparatus, the annealing apparatus, and the physical property measuring apparatus are arranged along a transfer path between the unwinding roll and the winding roll. The physical property measuring device transmits a predetermined signal to the control device. The control device stops the operation of the film forming device when receiving a predetermined signal transmitted from the physical property measuring device.

  In the thin film substrate manufacturing system according to the present application, the control device sets annealing conditions for the annealing device. The control device changes the annealing condition of the annealing device when receiving a predetermined signal transmitted from the physical property measuring device.

  The thin film substrate manufacturing system according to the present application includes substrate transfer means for transferring the substrate. The control device for controlling the transfer speed of the substrate transfer means changes the transfer speed of the substrate transfer means when receiving a predetermined signal transmitted from the physical property measuring apparatus.

  According to the present invention, among the thin films formed on the substrate and the substrate surface, the thin film can be heated to a higher temperature.

1 is a block diagram of an annealing apparatus according to a first embodiment. 1 is a block diagram of a computer according to Embodiment 1. FIG. It is explanatory drawing which shows the frequency characteristic of the dielectric loss of PEDOT: PSS. 3 is a flowchart showing a procedure of annealing treatment of the annealing apparatus according to the first embodiment. 3 is a flowchart showing a procedure of annealing treatment of the annealing apparatus according to the first embodiment. 6 is a block diagram of a thin film substrate manufacturing system according to Embodiment 2. FIG. FIG. 6 is a block diagram of an annealing apparatus according to a second embodiment. FIG. 6 is a block diagram of a computer according to a second embodiment. 10 is a flowchart illustrating a procedure of processing executed by a control unit of a computer according to Embodiment 2. FIG. 6 is a block diagram of an annealing apparatus according to a third embodiment.

  Hereinafter, the present invention will be described in detail with reference to the drawings showing embodiments thereof. Note that the present invention is not limited to the following embodiments.

Embodiment 1
The first embodiment relates to an annealing apparatus that anneals a thin film formed on a substrate surface by induction heating of electromagnetic waves. The frequency for selectively heating the thin film on the substrate surface is calculated as the frequency of the electromagnetic wave applied to the sample. Then, the thin film is annealed using the electromagnetic wave having the calculated frequency.

  FIG. 1 is a block diagram of an annealing apparatus 1 according to the first embodiment. An annealing apparatus 1 according to Embodiment 1 includes a processing container 2, a gas introduction mechanism 3, an exhaust mechanism 4, a mounting table 5, a radiation thermometer 6, a thermoelectric conversion element control unit 7, an electromagnetic wave supply unit 8, and a computer 9. The annealing apparatus 1 may not include the computer 9 by externally attaching the computer 9.

The processing container 2 is formed in a rectangular parallelepiped shape with aluminum, for example, and is grounded. A ceiling portion of the processing container 2 is opened, and a top plate 22 is airtightly provided in the opening portion via a seal member 21. The material of the top plate 22 is, for example, quartz, aluminum nitride or the like.
In addition, the shape of the processing container 2 is not limited to a rectangular parallelepiped shape whose upper portion is opened, and may be a columnar shape or a box shape.

An opening 23 is provided on the side wall of the processing container 2, and a gate valve 24 that opens and closes the opening 23 when the substrate K and the thin film H of the sample S are carried into and out of the processing container 2 is provided.
An exhaust port 25 connected to the exhaust mechanism 4 is provided at the peripheral edge of the bottom of the processing container 2.

The gas introduction mechanism 3 includes two gas nozzles 31 </ b> A and 31 </ b> B that penetrate the side wall of the processing container 2, and supplies a gas necessary for processing to the processing container 2 from a gas supply source (not shown). The gas here is, for example, an inert gas such as argon or helium, nitrogen, or the like.
The number of gas nozzles 31A and 31B is not limited to two, and may be increased or decreased as appropriate.

  The exhaust mechanism 4 includes an exhaust passage 41 through which exhaust flows, a pressure control valve 42 that controls the exhaust pressure, and an exhaust pump 43 that exhausts the atmosphere inside the processing container 2. The exhaust pump 43 can exhaust the atmosphere inside the processing container 2 to a reduced pressure level including a vacuum via the exhaust passage 41 and the pressure control valve 42.

The mounting table 5 is airtightly attached to an opening formed at the bottom of the processing container 2 with a seal member 26 interposed therebetween. The mounting table 5 is grounded.
The mounting table 5 includes a mounting table main body 51, a thermoelectric conversion element 52, and a mounting plate 53. A thermoelectric conversion element 52 is disposed on the mounting table main body 51, and a mounting plate 53 is disposed on the thermoelectric conversion element 52. On the mounting plate 53, the substrate K on which the thin film H to be annealed is formed is mounted.

  The radiation thermometer 6 includes a radiation thermometer main body 61 and an optical fiber 62 and measures the temperature of the mounting plate 53. The temperature of the mounting plate 53 measured by the radiation thermometer 6 is transmitted to the computer 9. The computer 9 that has received the temperature of the mounting plate 53 converts the temperature of the mounting plate 53 into the temperature of the thin film H in consideration of the temperature gradient between the mounting plate 53 and the thin film H.

A through hole 511 is formed in the mounting table main body 51 so as to vertically penetrate from the upper surface to the lower surface, and the optical fiber 62 is inserted in the through hole 511 in an airtight manner. The optical fiber 62 penetrates the lower surface of the mounting table main body 51 from directly below the lower surface of the mounting plate 53 and extends downward, and is connected to a radiation thermometer main body 61 provided outside the processing container 2. The radiation thermometer 6 is configured to be able to measure the temperature of the mounting plate 53 by incorporating the radiation light from the mounting plate 53 into the optical fiber 62.
In addition, the through-hole which penetrates the side wall of the processing container 2 may be provided, and the radiant light from the direct thin film H inserted airtightly through the through-hole may be taken into the optical fiber. Thereby, the temperature of the thin film H can be directly measured.

  The thermoelectric conversion element 52 is a plate-like cooling means for cooling the substrate K, and for example, a Peltier element is used. The Peltier element is a plate-like semiconductor element that utilizes the Peltier effect, and generates heat on one side and absorbs heat on the other side when a direct current is passed. Here, heat is absorbed on the upper surface of the thermoelectric conversion element 52 close to the substrate K, and the substrate K is cooled. On the other hand, heat is generated on the lower surface of the thermoelectric conversion element 52.

  The thermoelectric conversion element 52 is electrically connected to the thermoelectric conversion element control unit 7 provided outside the processing container 2 via a lead wire 71. The thermoelectric conversion element control unit 7 controls the direction and magnitude of the current supplied to the thermoelectric conversion element 52 during annealing. The thermoelectric conversion element 52 can also serve as a heating means for heating the substrate K by reversing the direction of the current flowing through the thermoelectric conversion element 52 by the thermoelectric conversion element control unit 7.

A coolant channel 512 is formed along a surface substantially parallel to the upper surface of the mounting table main body 51 in the upper portion of the mounting table main body 51 facing the lower surface of the thermoelectric conversion element 52. The refrigerant channel 512 is connected to a refrigerant circulator 515 that supplies a refrigerant via a refrigerant introduction pipe 513 and a refrigerant discharge pipe 514. When the refrigerant circulator 515 is operated, the refrigerant circulates and circulates through the refrigerant flow path 512 at the time of annealing, and the refrigerant takes away heat generated on the lower surface of the thermoelectric conversion element 52. Thereby, the cooling efficiency of the thermoelectric conversion element 52 improves.
Except for the thermoelectric conversion element 52, the cooling means for cooling the substrate K may be only the refrigerant circulation by the refrigerant circulator 515. The cooling means for cooling the substrate K may be a radiator.
It is also possible to circulate and circulate a high-temperature heating medium in the refrigerant flow path 512.

The mounting plate 53 is manufactured from a material such as silicon oxide, aluminum nitride, silicon carbide, germanium, or silicon.
The mounting table 53 may not be provided on the mounting table 5, and the substrate K may be directly mounted on the thermoelectric conversion element 52.

The electromagnetic wave supply unit 8 is provided above the top plate 22 of the processing container 2.
The electromagnetic wave supply unit 8 includes an electromagnetic wave generation source 81, a waveguide 82, and an incident antenna 83. One end of the waveguide 82 is connected to the electromagnetic wave generation source 81, and the other end of the waveguide 82 is connected to the incident antenna 83.

  As the electromagnetic wave generation source 81, for example, a gyrotron or a magnetron can be used. The gyrotron generally generates electromagnetic waves from millimeter waves to submillimeter waves. A magnetron generates a centimeter wave electromagnetic wave. The electromagnetic wave generation source 81 outputs the generated electromagnetic wave to the waveguide 82.

  The waveguide 82 is a metal tube that propagates the electromagnetic wave generated by the electromagnetic wave generation source 81 to the incident antenna 83, and has a circular or rectangular cross-sectional shape.

The incident antenna 83 is a plate provided on the top surface of the top plate 22 and is, for example, a copper plate or an aluminum plate whose surface is silver-plated. The incident antenna 83 is provided with a plurality of specular reflection lenses and reflection mirrors (not shown), and is configured to reflect and introduce the electromagnetic wave guided from the waveguide 82 toward the processing space of the processing container 2. ing.
The incident antenna 83 may be provided on the side surface of the processing container 2.

The computer 9 controls the operation of the annealing apparatus 1 as a whole.
FIG. 2 is a block diagram of the computer 9 according to the first embodiment.
The computer 9 includes a control unit 91, a ROM (Read Only Memory) 92, a RAM (Random Access Memory) 93, a communication unit 94, an operation unit 95, a display unit 96, an external interface 97, and a timer 98.

  Various programs are stored in the ROM 92. One of these programs causes the control unit 91 to calculate the most appropriate frequency as the frequency of the electromagnetic wave applied to the thin film H, for example.

  The control unit 91 reads a program from the ROM 92 and executes various processes. For example, the control unit 91 controls the supply of gas introduced into the processing container 2 by the gas introduction mechanism 3 and the gas flow rate. The control unit 91 controls the electromagnetic wave generated by the electromagnetic wave supply unit 8 and the power supplied to the electromagnetic wave supply unit 8. The control unit 91 controls the annealing temperature based on the signal from the radiation thermometer 6.

The RAM 93 temporarily records work variables, measurement data, and the like.
The communication unit 94 receives signals or data transmitted from each component of the annealing apparatus 1. In addition, the communication unit 94 transmits a command from the control unit 91 to each component of the annealing apparatus 1.

  The operation unit 95 includes input devices such as a keyboard and a mouse, and the user operates the computer 9 via the operation unit 95 and the communication unit 94. A user can operate the annealing apparatus 1 via the operation unit 95. The display unit 96 displays data input via the communication unit 94 and the operation unit 95, calculation results executed by the control unit 91, and the like.

The external interface 97 is an interface for exchanging information with a portable recording medium 1A such as a USB (Universal Serial Bus) memory or a CD-ROM (Compact Disc-Read Only Memory). The external interface 97 is also an interface that can be connected to a communication network N such as the Internet.
The timer 98 transmits the time count to the control unit 91 as a signal.

  Various programs for operating the annealing apparatus 1 according to the first embodiment may be recorded in the RAM 93 by causing the external interface 97 to read the portable recording medium 1A. The various programs can also be downloaded from another server computer (not shown) connected via the external interface 97 and a communication network N such as the Internet.

The program for calculating the frequency of the electromagnetic wave applied to the thin film H is to calculate the frequency of the electromagnetic wave using the thickness of the thin film H to be annealed as the penetration depth. The penetration depth means that when electromagnetic waves are incident on a conductive homogeneous medium vertically and propagate while exponentially decaying in the medium, the electromagnetic wave intensity is attenuated to 1 / e (about 37%) of the incident intensity. It is the depth of time.
The penetration depth is expressed by equation (1).

Where δ is the penetration depth, ρ is the resistivity, μ is the relative permeability, and f is the frequency of the electromagnetic wave.
When μ is a non-magnetic material, μ = 1. Since the film material handled in the first embodiment is a non-magnetic material, μ is fixed to 1.

  The substrate K targeted in the first embodiment is, for example, PET (polyethylene terephthalate), PEN (polyethylene naphthalate), PC (polycarbonate), or the like. The glass transition points of these plastic substrate materials are 100, 155, and 145 ° C., respectively. Here, a PET substrate is used.

  The thin film H targeted in the first embodiment is, for example, PEDOT: PSS. The annealing temperature of PEDOT: PSS is about 200 ° C., which is higher than the glass transition point of PET. Therefore, when the PEDOT: PSS thin film H is annealed by a conventional annealing method using a lamp or the like, the PET substrate is deformed.

  However, the penetration depth of the PET substrate with respect to electromagnetic waves of centimeter waves, millimeter waves, and submillimeter waves is much deeper than the penetration depth of the thin film H. Therefore, the frequency of the electromagnetic wave that almost passes through the PET substrate and passes through the thin film H of PEDOT: PSS only to the depth of the film thickness is calculated. Specifically, the frequency is calculated by substituting the film thickness into the penetration depth of the equation (1) and the resistivity of the thin film H into the resistivity. When the electromagnetic wave having the obtained frequency is a millimeter wave or a submillimeter wave, the annealing apparatus 1 in which a gyroton is mounted on the electromagnetic wave generation source 81 is used. When the electromagnetic wave having the obtained frequency is a centimeter wave, the annealing apparatus 1 having a magnetron mounted on the electromagnetic wave generation source 81 is used.

  In calculating the frequency of the electromagnetic wave, the film thickness of the thin film H and the penetration depth were assumed to be equal. However, for example, the thickness of the thin film H may be changed as appropriate, such as 90% or 110% of the penetration depth, and the thickness of the thin film H and the penetration depth are not limited to the same.

Next, the operation of the annealing apparatus 1 according to the first embodiment will be described.
Table 1 is an example of calculating the frequency for two types of PEDOT: PSS films.

A is an example when 11247 nm is selected as the film thickness and the resistivity is 5.0 × 10 ⁻³ Ωcm, and the frequency is 1.0 × 10 ¹¹ Hz. B is an example in the case where 1125 nm and a resistivity of 5.0 × 10 ⁻³ Ωcm are selected as the film thickness, and the frequency is 1.0 × 10 ¹³ Hz.

The thickness and resistivity of the thin film H are substituted into the computer 9 from the operation unit 95.
In the case of A in Table 1, the control unit 91 calculates 100 GHz (gigahertz) as a preferable frequency for measurement. Since 100 GHz corresponds to the frequency of the millimeter wave, the user uses the annealing apparatus 1 in which the gyrotron is mounted on the electromagnetic wave generation source 81 from the approximate frequency calculated in advance.
In the case of B in Table 1, the control unit 91 calculates 10 THz (terahertz) as a preferable frequency for measurement. Since 10 THz corresponds to the frequency of the submillimeter wave, the user uses the annealing apparatus 1 in which the gyrotron is mounted on the electromagnetic wave generation source 81 from the approximate frequency calculated in advance.

  FIG. 3 is an explanatory diagram showing frequency characteristics of dielectric loss of PEDOT: PSS. The vertical axis represents dielectric loss, and the horizontal axis represents frequency. The absorbed energy of electromagnetic waves is proportional to the dielectric loss that is the product of the relative dielectric constant and the dielectric loss tangent. As shown in FIG. 3, in the case of PEDOT: PSS, the maximum value of the dielectric loss is around 100 GHz. Therefore, as in the case of A in Table 1, when the thickness of the PEDOT: PSS thin film is set to 11 μm, the calculated frequency is 100 GHz, and the most efficient annealing can be performed. On the other hand, even if the PET substrate is irradiated with an electromagnetic wave of around 100 GHz, it is hardly heated because the penetration depth is deep, and the temperature of the PET substrate does not exceed the glass transition point.

Hereinafter, the case of A in Table 1 will be described.
The gate valve 24 is opened, and the PET substrate on which the PEDOT: PSS thin film H is formed is placed on the placement plate 53 by a conveying means (not shown). The gate valve 24 is closed and the processing container 2 is sealed. The thickness and resistivity of the thin film H to be annealed are input from the operation unit 95 to the computer 9. The controller 91 calculates the frequency of the electromagnetic wave based on the thickness and resistivity of the thin film H.

  The controller 91 sets the frequency of the electromagnetic wave generated by the electromagnetic wave generation source 81 to 100 GHz based on the calculated value. The controller 91 sets the intensity of the electromagnetic wave generated by the electromagnetic wave generation source 81. The controller 91 sets the annealing time and the processing pressure. The control unit 91 exhausts the inside of the processing container 2 by the exhaust mechanism 4 and introduces an inert gas or the like into the processing container 2 from the gas nozzles 31 </ b> A and 31 </ b> B of the gas introduction mechanism 3.

  The controller 91 starts an annealing process. That is, the control unit 91 generates an electromagnetic wave having a frequency set in the electromagnetic wave generation source 81. The control unit 91 operates the refrigerant circulator 515 to cool the mounting table body 51 and cools the substrate K by the thermoelectric conversion element 52 via the thermoelectric conversion element control unit 7. The controller 91 starts controlling the annealing temperature via the radiation thermometer 6. The annealing temperature is controlled by adjusting the intensity of electromagnetic waves.

  The electromagnetic wave generated by the electromagnetic wave generation source 81 is guided to the incident antenna 83 through the waveguide 82. The electromagnetic wave guided to the incident antenna 83 is reflected by the incident antenna 83 and supplied into the processing container 2. The electromagnetic wave supplied into the processing container 2 is applied to the thin film H and the substrate K.

  When the controller 91 determines that the annealing time has ended, the controller 91 stops driving the electromagnetic wave generation source 81. The controller 91 stops the control of the annealing temperature. The controller 91 waits for the thin film H to cool down and stops the introduction of the inert gas or the like by the gas introduction mechanism 3. The controller 91 stops the exhaust by the exhaust mechanism 4. The control unit 91 stops supplying current to the thermoelectric conversion element 52 via the thermoelectric conversion element control unit 7. The controller 91 stops the refrigerant circulator 515. That is, the controller 91 stops cooling the substrate K.

  The gate valve 24 is opened, and the sample on the mounting plate 53 is taken out of the processing container 2 by a conveying means (not shown). The gate valve 24 is closed and the processing container 2 is sealed.

4 and 5 are flowcharts showing the procedure of the annealing process of the annealing apparatus 1 according to the first embodiment.
The controller 91 receives the film thickness of the thin film H and the resistivity of the thin film H (step S101). The control unit 91 calculates the frequency of the electromagnetic wave applied to the sample from the equation (1) based on the received thickness of the thin film H and the resistivity of the thin film H (step S102). The control unit 91 sets the calculated frequency to the frequency of the electromagnetic wave generated by the electromagnetic wave generation source 81 (step S103). The controller 91 sets the intensity of the electromagnetic wave generated by the electromagnetic wave generation source 81 (step S104). The controller 91 sets an annealing time (step S105). The controller 91 sets a processing pressure (step S106).

  The control unit 91 exhausts the inside of the processing container 2 (step S107). The controller 91 introduces an inert gas or the like from the gas nozzles 31A and 31B into the processing container 2 (step S108). The controller 91 causes the electromagnetic wave generation source 81 to generate an electromagnetic wave (step S109). The control unit 91 operates the refrigerant circulator 515 to cool the mounting table main body 51 and starts cooling the substrate K by the thermoelectric conversion element 52 via the thermoelectric conversion element control unit 7 (step S110). The controller 91 starts controlling the annealing temperature (step S111).

  The controller 91 determines whether or not the annealing time has elapsed based on the timer 98 (step S112). When it is determined that the annealing time has not elapsed (step S112: NO), the controller 91 returns the control to step S112. When the controller 91 determines that the annealing time has elapsed (step S112: YES), the controller 91 stops the generation of electromagnetic waves by the electromagnetic wave generation source 81 (step S113). The controller 91 stops the control of the annealing temperature (step S114). The controller 91 stops the introduction of an inert gas or the like by the gas introduction mechanism 3 (Step S115). The controller 91 stops the exhaust by the exhaust mechanism 4 (step S116). The controller 91 stops the cooling of the substrate K (step S117) and ends the process.

  In step S101, the control unit 91 receives the resistivity of the thin film H. However, the resistivity of various materials may be recorded in the ROM 92 in advance, and the control unit 91 may read the resistivity of the thin film H from the ROM 92. In such a case, the control unit 91 receives the material of the thin film H in step S101, and reads the resistivity of the thin film H from the ROM 92 based on the received material of the thin film H.

  In step S102, the control unit 91 calculates the frequency of the electromagnetic wave applied to the sample from Equation (1) based on the received film thickness of the thin film H and the resistivity of the thin film H. However, the user may calculate the frequency of the electromagnetic wave applied to the sample from Equation (1) based on the film thickness of the thin film H and the resistivity of the thin film H, and the control unit 91 may receive the frequency input from the user. In such a case, the processing of the control unit 91 in step S101 and step S102 is processing for receiving a frequency. In step S103, the control unit 91 sets the received frequency to the frequency of the electromagnetic wave generated by the electromagnetic wave generation source 81.

  Table 2 is an example in which the penetration depth was estimated for the inorganic conductive material and the semiconductor material.

The silver of C is an example when a film thickness of 1948 nm and a resistivity of 1.5 × 10 ⁻⁶ Ωcm is selected, and the frequency is 1.0 × 10 ⁹ Hz. Silver of D is an example in which a film thickness of 195 nm and a resistivity of 1.5 × 10 ⁻⁶ Ωcm are selected, and the frequency is 1.0 × 10 ¹¹ Hz.
The copper E is an example in which a film thickness of 2012 nm and a resistivity of 1.6 × 10 ⁻⁶ Ωcm is selected, and the frequency is 1.0 × 10 ⁹ Hz. The copper of F is an example when the film thickness is 201 nm and the resistivity is 1.6 × 10 ⁻⁶ Ωcm, and the frequency is 1.0 × 10 ¹¹ Hz.
The aluminum of G is an example in which a film thickness of 2515 nm and a resistivity of 2.5 × 10 ⁻⁶ Ωcm are selected, and the frequency is 1.0 × 10 ⁹ Hz. The aluminum of H is an example when the film thickness is 252 nm and the resistivity is 2.5 × 10 ⁻⁶ Ωcm, and the frequency is 1.0 × 10 ¹¹ Hz.
The silicon of J is an example when the film thickness is 5030 nm and the resistivity is 1.0 × 10 ⁻¹ Ωcm, and the frequency is 1.0 × 10 ¹³ Hz.

In the case of C, E, and G in Table 2, the annealing apparatus 1 equipped with a magnetron that irradiates the electromagnetic wave generation source 81 with a centimeter wave electromagnetic wave is used. In the case of D, F, H, and J in Table 2, the annealing apparatus 1 equipped with a gyrotron that irradiates the electromagnetic wave generation source 81 with millimeter wave and submillimeter wave electromagnetic waves is used.
Moreover, according to the film thickness and resistivity of each thin film H, the electromagnetic wave of the frequency shown in Table 2 is selected, and it anneals. Thus, by selecting the frequency of the electromagnetic wave according to the difference in the film material, the thin film H can be selectively heated without making the temperature of the substrate K higher than the glass transition point.

According to the annealing apparatus 1 according to the first embodiment, the thin film H can be selectively heated at a higher temperature among the substrate K and the thin film H.
The substrate K and the thin film H are almost heated by irradiating the substrate K and the thin film H with a centimeter wave, a millimeter wave, or a submillimeter wave whose frequency corresponds to the penetration depth of the electromagnetic wave. Without this, the thin film H can be selectively heated.
Many inexpensive organic material substrates have a glass transition point below the annealing temperature of the organic conductive film material. Therefore, according to the annealing apparatus 1 according to the first embodiment, the thin film H of the organic conductive film material can be annealed without causing deformation of the organic material substrate, and the manufacturing cost of the organic device can be reduced. it can.

According to annealing apparatus 1 according to the first embodiment, temperature increase of substrate K can be suppressed by thermoelectric conversion element 52 and refrigerant circulator 515.
Even when electromagnetic waves are hardly absorbed by the substrate K, as the annealing time is prolonged, heat flows from the thin film H to the substrate K, and the temperature of the substrate K increases. However, by cooling the substrate K by the thermoelectric conversion element 52 and the refrigerant circulator 515, the transient state of thermal equilibrium can be prolonged. Film characteristics such as electrical conductivity are improved as the annealing temperature is higher and the annealing time is longer. Therefore, the cooling of the substrate K contributes to the improvement of the film characteristics.

Embodiment 2
The second embodiment relates to a thin film substrate manufacturing system in which a film forming apparatus, an annealing apparatus, and a physical property measuring apparatus are incorporated in a roll-to-roll manufacturing line for forming a thin film H on a flexible substrate K.

The board | substrate K made into object in Embodiment 2 is a film-like PET board | substrate, a PEN board | substrate, etc., for example.
The target thin film H in the second embodiment is a thin film H such as PEDOT: PSS, silylethyne-substituted pentacene, or poly (3-alkylthiophene).

FIG. 6 is a block diagram of the thin film substrate manufacturing system 100 according to the second embodiment.
The thin film substrate manufacturing system 100 includes a substrate transfer unit 11, a film forming device 12, an annealing device 10, a physical property measuring device 13, and a computer 90.
The film forming apparatus 12, the annealing apparatus 10 and the physical property measuring apparatus 13 are arranged in this order from the upstream to the downstream of the transfer line by the substrate transfer unit 11.

The substrate transfer unit 11 includes an unwinding roll 111, a take-up roll 112, and transfer rolls 113 and 114 that transfer the substrate K. The substrate transfer unit 11 unwinds the substrate K wound around the unwinding roll 111 at an appropriate tension and speed, and winds the thin film substrate formed by the film forming apparatus 12 and the annealing apparatus 10 onto the winding roll 112. The transfer rolls 113 and 114 transfer the substrate K from upstream to downstream by rotational driving. The operation of the substrate transfer unit 11 is continuous or discontinuous.
The substrate transfer unit 11 may not include the unwinding roll 111 and the winding roll 112. In such a case, a rotation driving unit that rotates the unwinding roll 111 and the winding roll 112 is separately prepared.

Although two transfer rolls 113 and 114 are illustrated in FIG. 6, the number of transfer rolls 113 and 114 is an example, and can be increased or decreased as appropriate. The substrate transfer unit 11 may include a plurality of pressing rolls that sandwich the substrate K between the transfer rolls 113 and 114 in order to improve the transfer efficiency of the substrate K.
In FIG. 6, the substrate transfer unit 11 holds the width direction of the substrate K in the horizontal direction and transfers the substrate K in the horizontal direction. However, the substrate transfer unit 11 may transfer the substrate K in the vertical direction while holding the width direction of the substrate K in the vertical direction.

  The film forming apparatus 12 is a pattern forming apparatus that forms a film pattern on the surface of the substrate K by printing, for example. The target of pattern formation by printing includes source / drain printing, semiconductor printing, gate printing, and the like. The film forming apparatus 12 may be a CVD apparatus, a PVD apparatus, or the like that deposits a material on a substrate K from a gas.

Annealing apparatus 10 is different from annealing apparatus 1 according to the first embodiment in that it corresponds to a roll-to-roll system.
FIG. 7 is a block diagram of annealing apparatus 10 according to the second embodiment. Here, parts of annealing apparatus 10 that are different from annealing apparatus 1 according to the first embodiment will be described.

The annealing apparatus 10 does not include the opening 23 and the gate valve 24.
At the opposite position of the side wall of the processing vessel 2, a carry-in port 27 for carrying in the substrate K and the thin film H before annealing and a carry-out port 28 for carrying out the substrate K and the thin film H after annealing are opened. The carry-in port 27 and the carry-out port 28 each have a slit shape longer than the width of the substrate K, and are provided at substantially the same height.
Shutters 27A and 28A are provided at the carry-in port 27 and the carry-out port 28, respectively. The shutters 27 </ b> A and 28 </ b> A shield the electromagnetic wave and gas inside the processing container 2 from leaking outside when the substrate transfer unit 11 stops transferring the substrate K and the substrate K and the thin film H are irradiated with electromagnetic waves. The shutters 27A and 28A are each made of a soft metal, such as indium or copper, and press the substrate K when the substrate transfer unit 11 stops the transfer of the substrate K.

  The physical property measuring device 13 includes a terahertz spectroscopic device, a film thickness measuring device, and an infrared spectroscopic device. The terahertz spectrometer measures the transmittance or reflectance of the terahertz wave with respect to the thin film H. The film thickness measuring device measures the thickness of the thin film H and transmits the measured thickness of the thin film H to the terahertz spectrometer. The terahertz spectrometer receives the thickness of the thin film H from the film thickness measuring device. The infrared spectrometer measures the reflectance of the infrared region with respect to the thin film H, and transmits the measured reflectance of the infrared region to the terahertz spectrometer. The terahertz spectrometer receives the infrared reflectance of the thin film H from the infrared spectrometer.

  The terahertz spectrometer is based on the transmittance or reflectance of the terahertz wave, the thickness of the thin film H, the reflectance in the infrared region, and the like, such as the complex refractive index, complex dielectric constant, complex electrical conductivity, and carrier mobility of the thin film H. Calculate physical properties. The physical property measuring device 13 or the terahertz spectrometer transmits the calculated physical property value of the thin film H to the computer 90.

FIG. 8 is a block diagram of a computer 90 according to the second embodiment.
The configuration of the computer 90 is the same as the configuration of the computer 9 included in the annealing apparatus 1 according to the first embodiment. Note that the computer 90 may be substituted by the computer 9 included in the annealing apparatus 10.
The computer 90 is electrically connected to the substrate transfer unit 11, the film forming apparatus 12, the annealing apparatus 10, and the physical property measuring apparatus 13, and controls these apparatuses.

Next, the operation of the thin film substrate manufacturing system 100 according to Embodiment 2 will be described.
First, in preparation for operating the thin film substrate manufacturing system 100, the frequency of the electromagnetic wave generated by the electromagnetic wave generation source 81 of the annealing apparatus 10 is set in the computer 90 in advance.

  The resistivity and film thickness of the thin film H are input to the computer 90 from the operation unit 950. The control unit 910 of the computer 90 transmits the acquired resistivity and film thickness of the thin film H to the computer 9 of the annealing apparatus 10. The computer 9 receives the resistivity and film thickness of the thin film H, and calculates the frequency of electromagnetic waves suitable for annealing. The computer 90 sets the calculated frequency to the frequency of the electromagnetic wave generated by the electromagnetic wave generation source 81.

  The roll of the substrate K is attached to the unwinding roll 111, and the operation of the thin film substrate manufacturing system 100 is started.

FIG. 9 is a flowchart illustrating a procedure of processing executed by the control unit 910 of the computer 90 according to the second embodiment.
The control unit 910 starts the operations of the substrate transfer unit 11, the film forming apparatus 12, the annealing apparatus 10, and the physical property measuring apparatus 13 (Step S201). The specific contents are as follows.
The control unit 910 operates the substrate transfer unit 11 to unwind the substrate K to the roll-to-roll production line. The control unit 910 operates the film forming apparatus 12 to print a pattern on the surface of the substrate K. The controller 910 causes the annealing apparatus 10 to anneal the thin film H formed by the film forming apparatus 12 via the computer 9. The control unit 910 causes the physical property measuring device 13 to measure the physical properties of the thin film H annealed by the annealing device 10. The controller 910 causes the manufactured thin film substrate to be taken up by the take-up roll 112.

The physical property measuring device 13 transmits the measured physical property value to the computer 90.
The control unit 910 acquires the physical property value of the thin film H from the physical property measuring device 13 (step S202). The control unit 910 determines whether the physical property value of the thin film H is within the range of the manufacturing standard (step S203). When the control unit 910 determines that the physical property value of the thin film H is within the range of the manufacturing standard (step S203: YES), the control unit 910 returns the control to step S201. When the control unit 910 determines that the physical property value of the thin film H is not within the range of the manufacturing standard (step S203: NO), the operation of the substrate transfer unit 11, the film forming apparatus 12, the annealing apparatus 10, and the physical property measuring apparatus 13 is performed. Stop (step S204).
The control unit 910 executes the above steps continuously in multitasking.
When the operations of the substrate transfer unit 11, the film forming device 12, the annealing device 10, and the physical property measuring device 13 are stopped, the user removes the non-manufacturing thin film substrate from the winding roll 112.

  The control unit 910 waits for an instruction from the user. The user instructs the computer 90 whether or not to resume manufacturing the thin film substrate. The control unit 910 receives an instruction from the user, and determines whether or not to resume the operations of the substrate transfer unit 11, the film forming apparatus 12, the annealing apparatus 10, and the physical property measuring apparatus 13 (step S205). When the operation is restarted (step S205: YES), the control unit 910 causes the film forming apparatus 12 to change the film forming conditions or causes the annealing apparatus 10 to change the annealing conditions (step S206), and performs processing in step S201. return. The change of the film forming conditions here is to change pattern forming conditions such as resist conditions and printing speed, for example. The change of the annealing conditions here is, for example, to set the intensity of the electromagnetic wave to a value that is larger by a predetermined value. Alternatively, the annealing condition is changed by changing the annealing time. When the operation is not resumed (step S205: NO), the control unit 910 ends the process.

  According to the thin film substrate manufacturing system 100 according to Embodiment 2, the thin film substrate can be continuously manufactured by the roll-to-roll method. In addition, by incorporating the physical property measuring device 13 in the roll-to-roll production line, the production line can be stopped when the quality of the thin film substrate being produced is out of the production standard. Thereby, the yield can be improved.

  According to the thin film substrate manufacturing system 100 according to the second embodiment, when the quality of the thin film substrate being manufactured is out of the manufacturing standards, the manufacturing conditions of the thin film substrate are optimized in a short time, and then the manufacturing is resumed. Can do. Optimizing the manufacturing conditions of the thin film substrate is, for example, changing the intensity of electromagnetic waves. Since the thin film substrate manufacturing system 100 according to the second embodiment has such a feedback function, the production efficiency of the thin film substrate can be improved.

  The second embodiment is as described above, and the other parts are the same as those of the first embodiment. Therefore, the corresponding parts are denoted by the same reference numerals, and detailed description thereof is omitted.

Embodiment 3
The third embodiment relates to a mode in which the annealing apparatus 10 of the thin film substrate manufacturing system 100 according to the second embodiment is replaced with another annealing apparatus.

FIG. 10 is a block diagram of annealing apparatus 20 according to the third embodiment.
The annealing apparatus 20 according to the third embodiment does not include the mounting table 5 of the annealing apparatus 10 according to the second embodiment, but includes a mounting roll 50 instead.
Further, the annealing apparatus 20 according to the third embodiment is different from the annealing apparatus 10 according to the second embodiment in that the optical fiber 62 of the radiation thermometer 6 receives radiation light from the substrate K.

The mounting roll 50 has a cylindrical shape or an elliptical column shape, and is attached so as to be partially inserted into an opening formed in the bottom of the processing container 2. The mounting roll 50 is grounded in a manner not shown. The mounting roll 50 is configured to rotate around an axis, and has a function of transferring the substrate K in contact with the side surface and a function of cooling the substrate K.
When the substrate transfer unit 11 stops the transfer of the substrate K and the substrate K and the thin film H are irradiated with electromagnetic waves, a shutter (not shown) is configured to close the gap between the mounting roll 50 and the bottom of the processing container 2. Has been. The shutter is made of a soft metal such as indium or copper, and when the substrate transfer unit 11 stops transferring the substrate K, it presses a part of the mounting roll 50 and a part of the bottom of the processing container 2. The shutter opens a gap between the placement roll 50 and the bottom of the processing container 2 when the substrate transfer unit 11 resumes the transfer of the substrate K.

  The mounting roll 50 includes a mounting roll body 510, a thermoelectric conversion element 520, and a mounting roll plate 530. A plurality of thermoelectric conversion elements 520 are disposed on the outer surface of the columnar mounting roll body 510, and a cylindrical mounting roll plate 530 is disposed on the outer surface of the thermoelectric conversion element 520. The substrate K is placed at the uppermost position of the placement roll plate 530.

A coolant channel 512 is formed along the cylindrical surface substantially parallel to the outer surface of the mounting table main body 510 at the edge of the mounting table main body 510 facing the inner surface of the thermoelectric conversion element 520. The refrigerant channel 512 is connected to a refrigerant circulator 515 that supplies a refrigerant via a refrigerant introduction pipe 513 and a refrigerant discharge pipe 514. By operating the refrigerant circulator 515, the refrigerant circulates through the refrigerant flow path 512 during annealing, and the refrigerant takes away heat generated on the inner surface of the thermoelectric conversion element 520. Thereby, the cooling efficiency of the thermoelectric conversion element 520 improves.
Note that it is also possible to circulate and circulate the heating medium through the refrigerant flow path 512.

The mounting roll plate 530 is made of a material such as silicon oxide, aluminum nitride, silicon carbide, germanium, or silicon.
In addition, the mounting roll plate 530 may not be provided on the mounting roll 50, and the substrate K may be directly mounted on the outer surface of the thermoelectric conversion element 520.

A through hole 29 is formed at the bottom of the processing container 2, and an optical fiber 62 is inserted into the through hole 29 in an airtight manner. The optical fiber 62 penetrates the bottom through the through hole 29, and one end thereof is connected to the radiation thermometer main body 61. The other end of the optical fiber 62 extends upward to just below the substrate K, and takes in the radiated light from the substrate K.
Thus, the radiation thermometer 6 of the annealing apparatus 20 measures the temperature of the substrate K. The temperature of the substrate K measured by the radiation thermometer 6 is transmitted as a signal to the computer 9 of the annealing apparatus 20. The computer 9 receives the signal from the radiation thermometer 6 and converts the temperature of the substrate K into the temperature of the thin film H.

  According to the annealing apparatus 20 according to the third embodiment, since the mounting roll 50 has a roll shape and rotates to transfer the substrate K, the substrate K can be smoothly moved corresponding to the roll-to-roll method. It is. Thereby, the thin film substrate manufacturing system 100 can efficiently and continuously produce thin film substrates. Since the mounting roll 50 includes the thermoelectric conversion element 520 that cools the substrate K and the coolant channel 512, the mounting roll 50 contributes to selective heating of the thin film H by cooling the substrate K.

  The third embodiment is as described above, and the other parts are the same as in the first or second embodiment. Therefore, the corresponding parts are denoted by the same reference numerals, and detailed description thereof is omitted.

DESCRIPTION OF SYMBOLS 1 Annealing apparatus 8 Electromagnetic wave supply part 81 Electromagnetic wave generation source 82 Waveguide 83 Incident antenna 91 Control part K Substrate H Thin film S Sample

Claims (11)

In an annealing apparatus that heats the substrate and the thin film formed on the surface of the substrate by irradiating with electromagnetic waves, and annealing the thin film,
Calculating means for calculating the frequency of electromagnetic waves applied to the substrate and the thin film based on the film thickness and resistivity of the given thin film;
An annealing apparatus comprising: an electromagnetic wave supplying unit that irradiates the substrate and the thin film with an electromagnetic wave having a frequency calculated by the calculating unit. The calculating means includes
The annealing apparatus according to claim 1, wherein the frequency of the electromagnetic wave is calculated so that a penetration depth of the electromagnetic wave with respect to the thin film corresponds to a film thickness of the thin film. The electromagnetic wave supply means includes
The annealing apparatus according to claim 1, wherein the thin film is heated to a higher temperature than the substrate. The annealing apparatus according to any one of claims 1 to 3, further comprising a cooling unit that cools the substrate. In the annealing method of annealing the thin film by heating the substrate and the thin film formed on the substrate surface by irradiating with electromagnetic waves,
Based on the film thickness and resistivity of the thin film, calculate the frequency of the electromagnetic wave irradiated to the substrate and the thin film,
An annealing method, wherein an electromagnetic wave having a calculated frequency is used to heat a thin film to a higher temperature than the substrate. The annealing method according to claim 5, wherein the substrate is made of an organic material. The annealing method according to claim 5 or 6, wherein the substrate is cooled. In the thin film substrate manufacturing system provided with a film forming apparatus for forming a thin film on the surface of the substrate in the process of unwinding the flexible substrate wound on the unwinding roll and winding it on the winding roll,
The annealing apparatus according to any one of claims 1 to 4, wherein the thin film formed by the film forming apparatus is annealed under an arbitrary annealing condition;
A thin film substrate manufacturing system comprising: a physical property measuring device for measuring physical properties of the annealed thin film. A control device that receives a signal from the physical property measuring device and controls the operation of the film forming device;
The film forming apparatus, the annealing apparatus, and the physical property measuring apparatus are disposed along a transfer path between the unwinding roll and the winding roll,
The physical property measuring apparatus is:
Transmission means for transmitting a predetermined signal to the control device;
The controller is
The thin film substrate manufacturing system according to claim 8, further comprising means for stopping the operation of the film forming apparatus when the predetermined signal transmitted by the transmitting means of the physical property measuring apparatus is received. The controller is
Annealing conditions of the annealing apparatus are set,
The thin film substrate manufacturing system according to claim 9, further comprising means for changing an annealing condition of the annealing apparatus when the predetermined signal transmitted by the transmitting means of the physical property measuring apparatus is received. Substrate transfer means for unwinding and transferring the substrate from an unwinding roll at an arbitrary transfer speed, and winding the thin film substrate having a thin film formed on the surface of the substrate on a winding roll;
The controller is
The transfer speed of the substrate transfer means is controlled,
11. The thin film substrate manufacturing method according to claim 9, further comprising means for changing a transfer speed of the substrate transfer unit when the predetermined signal transmitted by the transmission unit of the physical property measuring apparatus is received. system.

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