JP5070932B2 - Film temperature measuring apparatus and winding type vacuum film forming apparatus equipped with the same - Google Patents

Description

  The present invention relates to an apparatus for measuring the temperature of a traveling film when a film is formed on one surface of a film by a film forming apparatus, and a take-up vacuum film forming apparatus provided with the film temperature measuring apparatus.

  Conventionally, plastic films such as polyethylene terephthalate, polyimide, polyester, polyethylene, and nylon have been used as a base material for functional films coated with various coating materials to give various properties. In particular, in the field of electronic materials and packaging materials, a relatively thin film having a thickness of about several tens of μm is often used. With the expansion of application types of materials to be coated, functional films based on the above plastic films are used. It is expected to increase in the future.

  Various functional thin film production methods include various sputtering methods using a target such as metal or oxide, such as direct current magnetron sputtering, high frequency magnetron sputtering, magnetron sputtering in which high frequency RF is superimposed on direct current, and the targets are made to face each other. There is counter target sputtering. In addition, a reactive vapor deposition method by supplying a plasma beam to an oxide target arranged as an anode and evaporating a material evaporation source, or using gas plasma to convert some of the evaporated particles into ions or excited particles for activation. An ion plating method or the like for vapor deposition is used.

  In the above thin film manufacturing method, the characteristics of the functional thin film formed on the film often change depending on the temperature of the film serving as the substrate, and therefore the method for controlling the film temperature has been an important consideration. For example, in a single-wafer type vacuum film forming apparatus that forms a thin film under vacuum, a direct heating means such as a film or a film holder such as a nichrome wire, an infrared lamp, or a halogen lamp, and water, ethylene glycol, or a fluorocarbon refrigerant are used. The temperature of the film is adjusted by combining a cooling means for the film holder that flows and cools using surface contact, and a measuring means comprising various thermometers for measuring the film temperature.

  On the other hand, in a roll-up vacuum film forming apparatus that forms a film while transporting a web-like film continuously between two rolls, the film temperature is damaged when the thermometer is contacted. Have difficulty. Therefore, in many cases, as shown in FIG. 1, a large film forming drum 2 that is heated and cooled by a cooling medium is provided in the vacuum chamber 1, and the film 3 runs on the film forming drum 2 along with the rotation of the film forming drum 2. The temperature of the film 3 is controlled by controlling the liquid temperature of a cooling / heating medium that flows into the film formation drum 2 while forming the film.

  However, when measuring the temperature of the traveling film in this way, it is difficult to measure using a normal thermometer because the film is easily damaged by contact with the thermometer. In addition, even if an attempt is made to measure the temperature by bringing the thermometer into contact with the film, there is a problem that it is difficult to measure the temperature with high accuracy because the heat capacity is particularly small in a thin film.

  Therefore, it has been studied to measure the temperature of the traveling film in a non-contact manner using a radiation thermometer. That is, a winding vacuum that forms a thin film on a film while running the film between an unwinding roll and a winding roll by a roll-to-roll method without using a film-forming drum that can be heated and cooled by a cooling medium. Using a film deposition device, a radiation thermometer is placed in the space on the back side of the film (the side opposite to the surface on which the thin film is formed), and the temperature of the film being deposited is measured in a non-contact manner It is.

  In such a winding type vacuum film forming apparatus, the temperature of the film during running and film formation depends on the film forming conditions, and if the film temperature is too high, the film may be deformed or broken. is there. Usually, the temperature of the film is different at the beginning and the end of film formation, and in some cases, the temperature of the film may be different between the center and the end of the film. Furthermore, since the film characteristics may change depending on the temperature of the film, it is necessary to pay close attention to the temperature of the film.

  However, when the film temperature during film formation is measured from the back side opposite to the film formation side of the film running as described above, even if there is a space on the back side of the film, the member in the vacuum chamber In many cases, there is only one measurement point because there are many cases where the space is limited due to the arrangement or the introduction of a measurement device. Therefore, the temperature of the entire film cannot be known, and there has been a problem that accurate temperature control cannot be performed at the center and end of the film or at the beginning and end of film formation.

  Looking only at the temperature measurement technique of the film, for example, in Japanese Patent Laid-Open No. 11-333920 (Patent Document 1), in a method for producing a resin film having a stretching process after coating a coating on at least one side, By measuring the temperature of the film using a thermometer, after the drying process of the coating material and before the stretching process, it is continuously measured in the width direction of the film to grasp the drying state of the coating material, and the information is dried. It is described that the heating in the drying process is controlled by feeding back to the process, and the film is stretched after reaching a certain temperature or higher.

  JP 2000-187203 A (Patent Document 2) discloses that in the production of a biaxially stretched polyamide film, when the film is stretched in the longitudinal direction, it can be measured in the width direction immediately before the stretching point in the longitudinal direction. By installing a non-contact radiation thermometer and heating the film end by automatically changing the output of the heat source that heats the film end based on the measured temperature, the width direction after stretching in the longitudinal direction It has been proposed to produce a biaxially stretched polyamide film with excellent dimensional stability and small physical property difference in the width direction by reducing the difference in physical properties of the film between the center and the edge and stretching the uniaxially stretched film in the width direction. ing.

  Japanese Patent Laid-Open No. 2005-218686 (Patent Document 3) arranges a radiation thermometer capable of detecting infrared rays in a specific wavelength region outside the body of a dry sterilizer and generates it from a heated container. A dry sterilizer capable of accurately measuring the temperature of a container and facilitating maintenance by attaching a window made of a material capable of transmitting infrared in the wavelength range detected by a radiation thermometer among infrared rays to be measured Has been proposed. However, all of the above measuring methods are performed using a radiation thermometer in the atmosphere, and there is no description of measuring the temperature during film formation of a film running in a vacuum film forming apparatus.

JP-A-11-333920 JP 2000-187203 A JP 2005-218686 A

  In view of the above-described conventional circumstances, the present invention is a film that is being formed using a radiation thermometer while forming a film on a traveling film supported by two guide rolls in a take-up vacuum film forming apparatus. It is an object of the present invention to provide an apparatus capable of accurately measuring the temperature at a plurality of locations on a film when measuring the temperature of the film, and a take-up vacuum film forming apparatus equipped with the temperature measuring apparatus.

  In order to achieve the above object, the film temperature measuring apparatus provided by the present invention provides a film-to-film measuring surface opposite to the film-forming surface when forming a thin film on one surface of a traveling film by a roll-to-roll vacuum film forming apparatus. A temperature measuring device for measuring the temperature of the film from a surface with a radiation thermometer, a metal tube held movably on a wall portion of the film forming apparatus by a holding portion, and a radiation thermometer installed in the metal tube; , Equipped with a window provided in the metal tube and a reflector disposed inside the window of the metal tube, and infrared rays incident on the window of the metal tube from the film are reflected by the reflector and detected by a radiation thermometer Thus, the temperature of the film during film formation is measured.

  In the film temperature measuring device of the present invention, the holding portion of the metal tube is connected to a rotary cylinder and a linear cylinder, the metal tube is rotatable around the axis of the metal tube, and in the axial direction of the metal tube. It is preferably movable. Moreover, it is preferable that the outer peripheral part of the said metal pipe is water-cooled. Furthermore, it is preferable that the window member installed in the window portion is made of one kind selected from barium fluoride, calcium fluoride, and ZnSe.

  The present invention also provides a take-up vacuum film forming apparatus for forming a thin film on one surface of a film traveling by a roll-to-roll method, comprising the film temperature measuring device of the present invention described above. It is.

  In the winding type vacuum film forming apparatus of the present invention, the film temperature measured by the film temperature measuring device is fed back to the evaporation source or the power supply device of the electrode and the film transport device, and the input power and the film transport speed are The temperature of the film can be controlled by adjusting.

  According to the film temperature measuring apparatus of the present invention, the infrared temperature from the film is detected by a radiation thermometer through the window of the metal tube, and the temperature of the film being traveled and being deposited is accurately measured without contact. In addition, by installing a metal tube containing a radiation thermometer in a rotatable and axially movable manner, any number of films can be made from a single radiation thermometer and a single vacuum introduction port. The temperature at the location can be measured.

  Therefore, by providing this film temperature measuring device in a direct current magnetron sputtering device, a high-frequency magnetron sputtering device, a counter sputtering device, a reactive vapor deposition device, an ion plating device, etc., the temperature of the film serving as a base material is detailed. In the production of various functional thin films, it is easy to control the characteristics of the functional thin film formed on the film and to obtain a functional thin film with more stable characteristics. It is extremely useful.

  The film temperature measuring apparatus of the present invention will be specifically described with reference to FIGS. For example, as shown in FIG. 2, in a roll-to-roll type roll-up vacuum film forming apparatus, an evaporation source is formed on one surface of a film 4 running between two rolls (not shown) according to the film forming method. / A thin film is formed using the electrode 5. As for the evaporation source / electrode 5, the evaporation source is used in a resistance heating method or an electron beam evaporation method, and the electrode is used in a sputtering method using plasma, a plasma CVD method, an ion plating method, or the like.

  A metal tube 6 is movably installed on the back side opposite to the film formation surface of the film 4 on which the evaporation source / electrode 5 is installed, and the film is formed by a radiation thermometer 7 housed in the metal tube 6. Measure the temperature of 4. The metal tube 6 is held by the holding unit 9 on the wall 8 of the film forming apparatus and can be moved by an operation from the outside of the film forming apparatus. For example, the metal tube 6 can be rotated around the metal tube 6 by a rotary cylinder 10 and linear. The cylinder 11 is movable in the axial direction of the metal tube 6. Therefore, it is possible to measure temperatures at arbitrary plural positions of the traveling film 4 from the single radiation thermometer 7 and the single vacuum introduction port.

  For example, as shown in FIG. 3, a window portion 12 is provided at the tip of the metal tube 6 in which the radiation thermometer 7 is housed, and a reflecting mirror 13 is disposed inside the window portion 12. The window member provided in the window portion 12 is preferably one type selected from barium fluoride, calcium fluoride, and ZnSe. Then, the infrared ray incident on the window 12 of the metal tube 6 from the film 4 is reflected by the reflecting mirror 13 and detected by the radiation thermometer 7 to measure the temperature of the film 4 being formed. Yes. Note that reference numeral 15 in FIG. 3 denotes a deposition preventing plate for regulating the film formation region of the film 4.

  Furthermore, it is preferable that the outer periphery of the metal tube 6 containing the radiation thermometer 7 is water-cooled. In the process of forming a film on the film 4, not only the film 4 but also the metal tube 6 may be heated by the electrode / evaporation source 5. This makes it possible to eliminate the malfunction of the radiation thermometer 7 and to perform more accurate measurement.

  The radiation thermometer is preferably selected so that the emissivity of the film is as high as possible at the detection wavelength together with the detection wavelength of the radiation thermometer. This is because the film is not a complete absorber that absorbs all infrared rays from the outside like a complete blackbody radiator, but reflects, absorbs, and transmits part of the infrared wavelength. Moreover, each ratio is called a reflectance, an absorptivity, and a transmittance | permeability, and it is known that an absorptivity and an emissivity are equal among these. That is, there is a relationship of H = rH + aH + tH (where r + a + t = 1) between the total energy H of infrared rays incident on the resin film from the outside, the reflectance r, the absorption rate a, and the transmittance t, and the transmitted or reflected infrared rays. This is because it is desirable to make the inhibition factor as small as possible because energy also enters the radiation thermometer and inhibits accurate measurement.

  From the same concept, it is desirable that the radiation transmission window material of the radiation thermometer has as high a transmittance as possible at the detection wavelength. Specifically, the material of the window member installed in the window portion of the metal tube is preferably one selected from barium fluoride, calcium fluoride, and ZnSe. Also, it is desirable that the reflecting mirror has as high a reflectance as possible. For the reasons described above, the display value of the radiation thermometer is generally not accurate, so calibration is required.

  Usually, the calibration is performed as follows. That is, a film is attached to a take-up vacuum film forming apparatus, and a thermocouple is attached to the stopped film. In this state, a thin film is formed on the film, for example, by sputtering. At that time, using a radiation thermometer housed in a metal tube, the radiation at the window is guided by a reflecting mirror and detected to measure the temperature at the same place as the thermocouple. Adjust the input power to the electrode and obtain the measured value of the thermocouple and the display value of the radiation thermometer while the temperature of the thermocouple is stable. The calibration curve of the radiation thermometer can be obtained from the relationship between the measured value of the thermocouple thus obtained and the display value of the radiation thermometer.

  The film temperature measuring apparatus of the present invention can be installed in a direct current magnetron sputtering apparatus, a high-frequency magnetron sputtering apparatus, a counter sputtering apparatus, or a film forming apparatus using a reactive vapor deposition method or an ion plating method. According to the obtained roll-to-roll type vacuum film forming apparatus, the temperature of the film formed while moving can be accurately measured in a non-contact manner at a plurality of locations.

  In particular, the film temperature measured by the film temperature measuring device is fed back to the evaporation source or the electrode power supply device and the film transport device, and the temperature of the film being formed is adjusted by adjusting the input power and the film transport speed. It is possible to control in detail. As a result, since the film formation conditions can be optimized, the characteristics of the functional thin film formed on the film can be easily controlled, and a functional thin film with more stable characteristics can be obtained.

[Example 1]
A roll-to-roll type vacuum film forming apparatus equipped with the film temperature measuring device shown in FIGS. 2 and 3 is used, and a polyimide film (made by Toray DuPont, Kapton (registered by Toray DuPont) with a thickness of 262 mm is registered. Trademark)). A thermometer (Japan sensor, TMZ53-350F7-100N67M5-D, detection wavelength 7.9 μm) with a reflector is attached to the stopped film with a K thermocouple with a sheath diameter of 0.5 mm attached to the metal It was inserted into a tube and adjusted so that a place equivalent to a thermocouple could be measured through a window member made of barium fluoride.

  In this state, a copper thin film was formed on the film by sputtering. At that time, the input power to the sputtering electrode is adjusted, the measured value of the thermocouple and the display value of the radiation thermometer are obtained in a state where the temperature of the thermocouple is stable, and the relationship obtained is shown in FIG. The graph of FIG. 4 was used as a calibration curve for the radiation thermometer.

Subsequently, a copper thin film was formed on the film with a power of 10 W / cm ² by a sputtering method while running the film at a speed of 1.5 m / min by a roll-to-roll method. With the temperature stabilized, the rotary cylinder and linear cylinder were adjusted, and the film temperature at each measurement position shown in FIG. 5 was measured with a radiation thermometer. The obtained measurement results are shown in Table 1 below.

  As can be seen from Table 1 below, there was almost no temperature distribution in the film width direction (measurement positions B, D, E), but in the film length direction (measurement positions A, B, C), the film temperature was The temperature rose with the treatment and reached the highest temperature at the end of the treatment. Moreover, on the said conditions, the film formed into a film could be wound up stably, without deform | transforming or fracture | rupture.

[Example 2]
A copper thin film was formed on the film and the film temperature at that time was measured in the same manner as in Example 1 except that the film was run at a speed of 0.38 m / min. The obtained results are shown in Table 1 below.

  As can be seen from Table 1 below, there was almost no temperature distribution in the lateral direction of the film (measurement positions B, D, E), but in the film length direction (measurement positions A, B, C), the film temperature was It rose with the treatment, peaked near the middle of the treatment, and the temperature was almost constant at the end of the treatment.

  Further, the running speed of the film was changed to 1.5 m / min and 0.75 m / min in addition to the above 0.38 m / min, and a copper thin film was formed under the same conditions as above. At that time, the temperature of the film in the film length direction (measurement positions A, B, C) was measured, and the obtained results are shown in FIG. Moreover, the film formed into a film on any conditions was able to wind up stably, without deform | transforming and fracture | rupturing.

[Comparative Example 1]
A copper thin film was formed on the film in the same manner as in Example 1 except that the input power was 20 W / cm ² , and the film temperature at that time was measured. The obtained results are shown in Table 1 below.

  As can be seen from Table 1 below, there was almost no temperature distribution in the film width direction (measurement positions B, D, E), but in the film length direction (measurement positions A, B, C), the film temperature was It rose with the treatment and reached the highest temperature at the end of the treatment. Moreover, wrinkles were generated in the film in which the copper thin film was formed under the above conditions.

[Comparative Example 2]
A copper thin film was formed on the film in the same manner as in Example 1, except that the rotary cylinder and the linear cylinder were not used and only the temperature at the center of the film (measurement position B) was measured. The obtained results are shown in Table 1 below. The temperature of the film was measured only at measurement position B, and temperature data at other positions could not be acquired.

[Example 3]
In the same manner as in Example 1 above, a roll-to-roll type roll-up vacuum film forming apparatus equipped with the film temperature measuring device shown in FIGS. 2 and 3 was used, and a polyimide film having a thickness of 38 μm and a width of 262 mm A copper thin film was formed on the film with a power of 10 W / cm ² by a sputtering method while running Kapton (registered trademark, manufactured by Toray DuPont) at a speed of 1.5 m / min.

  At this time, in the same manner as in Example 1 above, the temperature of the running film is measured, and the measurement result is fed back to the power supply device of the target electrode and the film transport device, so that the film temperature becomes constant. In this way, film formation was continuously performed. As a result, the surface temperature of the film was controlled within 5 ° C. around 145 ° C. set in advance at the position B in FIG. 5, and the film formation could be continued stably in this temperature range.

It is a schematic sectional drawing which shows the specific example of the winding type vacuum film-forming apparatus provided with the conventional film-forming drum. It is a schematic perspective view which cuts and shows a part of principal part of the winding type vacuum film-forming apparatus provided with the film temperature measuring device of the present invention. 1 is a schematic plan view showing a specific example of a film temperature measuring device of the present invention with a part cut away. FIG. It is an example of the calibration curve of a radiation thermometer, and is a graph which shows the relationship between the measured value of a thermocouple, and the display value of a radiation thermometer. It is explanatory drawing which shows the temperature measurement position of a film. 6 is a graph showing measurement results of film temperature in Example 2.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Vacuum chamber 2 Film-forming drum 3, 4 Film 5 Electrode / evaporation source 6 Metal tube 7 Radiation thermometer 8 Wall part 9 Holding part 10 Rotary cylinder 11 Linear cylinder 12 Window part 13 Reflector 14 Water-cooling jacket 15 Adhesion board

Claims (5)

A temperature measuring device that measures the temperature of the film with a radiation thermometer from the surface opposite to the film-forming surface of the film when a thin film is formed on one surface of the traveling film by a roll-to-roll vacuum film forming device. A metal tube that is movably held by a holding unit on the wall of the film forming apparatus and whose outer peripheral part is water-cooled , a radiation thermometer installed in the metal tube, a window provided in the metal tube, A reflecting mirror disposed inside the window of the metal tube, and infrared rays incident on the window of the metal tube from the film are reflected by the reflecting mirror and detected by a radiation thermometer, thereby A film temperature measuring device for measuring temperature.   The holding portion of the metal tube is connected to a rotary cylinder and a linear cylinder, and the metal tube is rotatable around an axis of the metal tube and is movable in an axial direction of the metal tube. Item 2. The film temperature measuring device according to Item 1. The film temperature measuring device according to claim 1 or 2 , wherein the window member installed in the window portion is made of one selected from barium fluoride, calcium fluoride, and ZnSe. A roll-up vacuum film forming apparatus for forming a thin film on one surface of a film traveling by a roll-to-roll method, comprising the film temperature measuring device according to any one of claims 1 to 3 . The film temperature measured by the film temperature measuring device is fed back to an evaporation source or an electrode power supply device and a film transport device, and the film temperature is controlled by adjusting the input power and the film transport speed. The winding type vacuum film-forming apparatus according to claim 4 .

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