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WO1991008655A1 - Dispositif de traitement thermique et procede de sechage de pellicules minces fonctionnelles utilisant ledit dispositif - Google Patents

Dispositif de traitement thermique et procede de sechage de pellicules minces fonctionnelles utilisant ledit dispositif Download PDF

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Publication number
WO1991008655A1
WO1991008655A1 PCT/JP1990/001535 JP9001535W WO9108655A1 WO 1991008655 A1 WO1991008655 A1 WO 1991008655A1 JP 9001535 W JP9001535 W JP 9001535W WO 9108655 A1 WO9108655 A1 WO 9108655A1
Authority
WO
WIPO (PCT)
Prior art keywords
far
heat
heat treatment
direct
ceramic heater
Prior art date
Application number
PCT/JP1990/001535
Other languages
English (en)
Japanese (ja)
Inventor
Takeshi Yoshida
Original Assignee
Mita Industrial Co., Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Mita Industrial Co., Ltd. filed Critical Mita Industrial Co., Ltd.
Priority to KR1019910700785A priority Critical patent/KR920702179A/ko
Publication of WO1991008655A1 publication Critical patent/WO1991008655A1/fr

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B3/00—Drying solid materials or objects by processes involving the application of heat
    • F26B3/28—Drying solid materials or objects by processes involving the application of heat by radiation, e.g. from the sun
    • F26B3/30—Drying solid materials or objects by processes involving the application of heat by radiation, e.g. from the sun from infrared-emitting elements
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
    • H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
    • H05B3/141—Conductive ceramics, e.g. metal oxides, metal carbides, barium titanate, ferrites, zirconia, vitrous compounds
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/40—Heating elements having the shape of rods or tubes
    • H05B3/42—Heating elements having the shape of rods or tubes non-flexible

Definitions

  • the present invention relates to a heat treatment device for heat treating a columnar or tubular heat treatment object, and a method for drying a functional thin film using the same.
  • the heat treatment of the above-mentioned heat-treated object includes forming a functional thin film by drying a polymer-based coating liquid applied to the surface of a columnar or cylindrical substrate. Coating or vapor deposition formed on the surface of the substrate Examples include annealing of the coating, sintering of ceramics formed into columns or tubes, and quenching of metals.
  • the heat treatment apparatus used for heat treatment of the above-mentioned various heat-treating objects has a constant heat treatment object P as shown in FIGS.
  • a type is used in which heat is conveyed at a speed and passes through a heat treatment furnace H whose inside is heated to a predetermined temperature.
  • the means for heating the inside of the heat treatment furnace H to a predetermined temperature may be, for example, a type in which warm air is blown into the heat treatment furnace H, or a means arranged in the heat treatment furnace H as shown in the figure. Many h, h, etc. are used every day.
  • the surface of the coating film on the substrate is heated and dried before the inside, and the inside of the coating film is dried smoothly.
  • the coating film may have irregularities (so-called “skin skin”), peeling phenomenon, etc., and when the solvent evaporates from the inside of the coating film, defects such as bubbles, pinholes, and repelling of the coating film may occur.
  • a large amount of solvent remains in the layer and the performance becomes unstable.
  • the functional thin film is the photosensitive layer of the photosensitive drum, there is a problem that the sensitivity is poor, the stability of repeated exposure is deteriorated, and the layer is liable to be cracked or peeled off. is there.
  • Solvent remaining in the layer can be eliminated by storing the substrate after forming the functional thin film for a long period of time and allowing the solvent to evaporate spontaneously.However, the productivity is significantly reduced, and this poses a problem in terms of cost, etc. .
  • rapid heating may rather increase the stress inside the film, which may cause cracking or peeling.
  • rapid heating increases internal stress and causes cracks.
  • metal quenching rapid heating causes deformation due to uneven thermal expansion.
  • the inside of the heat treatment furnace is divided into a plurality of rooms, and the heating temperature set inside is gradually increased from the room on the entrance side toward the back, so that the object to be heat treated is The temperature is gradually increased by passing through each room in order from the room.
  • the above-mentioned conventional heat treatment furnace is used in order to increase productivity.
  • the so-called tunnel type in which the object to be heat-treated is heated and dried while being transported at a constant transport speed is generally used.
  • the heat-treating furnace becomes long, so there is a problem in terms of space and cost for installing the heat-treating furnace.
  • the main object of the present invention is to eliminate the need for a large-scale heat treatment furnace, to greatly reduce the space and cost for installation, heat treatment time, energy consumption, and the like, and to uniformly heat-treat the workpiece.
  • An object of the present invention is to provide a heat treatment apparatus capable of performing heat treatment.
  • Another object of the present invention is to provide a function capable of forming a uniform functional thin film having no defects such as fuse skin, air bubbles, pinholes, and repelling, and having a small internal stress, using the heat treatment apparatus. If a method for drying a conductive thin film is provided, it will be ⁇ .
  • a heat treatment including a cylindrical direct energization * far-infrared ceramic heater that heats the heat treatment object from the surroundings in a state where the heat treatment object is concentrically accommodated in a columnar or cylindrical shape
  • An apparatus is provided.
  • the heat treatment is performed in a state where the heat treatment object is concentrically accommodated in the cylindrical direct current / far infrared ray ceramics heater.
  • the above-described direct-current / far-infrared ceramic heater is configured by arranging a plurality of plate-shaped ceramic heaters in a cylindrical shape having a polygonal cross section, the manufacture is easy.
  • the heat treatment is performed by making the polygon have six or more corners, or by rotating the cylindrical direct-current / far-infrared ceramic heater and the object to be heat-treated relatively. Bias can be prevented.
  • a tube or rod-shaped direct current supply having a smaller outer diameter than the inner dimension of the object to be heat-treated Energization ⁇ Far-infrared ceramic mixer If placed concentrically within one day, the above-mentioned tubular object can be heat-treated from inside and outside.
  • a component in a specific wavelength region of the far-infrared rays emitted from the direct-current / far-infrared ceramic heater between the cylindrical direct-current / far-infrared ceramic heater and the object to be heated By inserting a wavelength cut filter that transmits only, for example, when the coating film is dried, it is directly energized.
  • the far-infrared rays emitted from the far-infrared ceramic heater are transmitted to the inside of the coating film.
  • the coating can be dried by irradiating only the obtained component in the specific wavelength region to the coating film.
  • a cylindrical direct-current / far-infrared ceramic heater is arranged with its axis oriented substantially vertically, and the inside of the direct-current / far-infrared ceramic heater is arranged.
  • a pallet is provided which moves while holding the object to be heat upright.
  • the pallet is provided with a step for holding the object to be heated while avoiding the non-heating regions at the upper and lower ends of the direct-current / far-infrared ceramic heater.
  • a blowing means for flowing air from the upper end to the lower end of the object to be heated may be disposed above the far-infrared ceramic heater directly energized.
  • the pallet is provided with a ventilation hole through which air from the blowing means passes.
  • a transport rail for transporting the above pallets is provided, a plurality of pallets are arranged on this transport rail, and a cylindrical direct energizing It is sufficient that the mixer is vertically moved with respect to the transport path of the object to be heat-treated by the transport rail.
  • a cooling means for cooling the cylindrical direct-current / far-infrared ceramic heater that is retracted from the transfer path of the object to be heat-treated by the rail is preferable to provide.
  • the outer circumference of the cylindrical direct-current / far-infrared ceramic heater is surrounded by a heat insulating material detachable from the direct-current / far-infrared ceramic heater, and the direct current- At the time of cooling by the cooling means of the far-infrared ray ceramic heater, the heat insulating material may be separated from the far-infrared ceramic heater and directly cooled.
  • a cooling means for cooling the heat insulating material a cooling pipe penetrated in the heat insulating material is preferably used.
  • two sets of cylindrical direct energizing, far-infrared ceramics heaters are alternately moved up and down with respect to the transport path of the object to be heat-treated by the transport rails.
  • the heat treatment target is arranged so as to heat it, and one of the direct energization and far-infrared ceramics heaters is used to heat the object to be heat-treated by one, while the other is directly energized and the far-infrared ceramics heater is cooled by cooling means It may be configured to cool.
  • the coating of the polymer-based coating solution formed on the surface of the columnar or cylindrical substrate is subjected to a predetermined natural drying, and then the above-mentioned direct energization is performed.
  • the temperature of the substrate is rapidly increased by using a heater to the glass transition temperature of the entire coating film after the film formation, which is determined by the composition and the amount of the polymer-based coating solution.
  • the surface of the coating film becomes more inward than the inside by gradually increasing the temperature or temporarily stopping the temperature after the glass transition temperature. It is possible to prevent the coating film from being dried first and to evenly dry the coating film to the inside.
  • FIG. 1 is a front view showing the configuration of a preferred heat treatment apparatus according to the present invention.
  • FIG. 2 is a perspective view showing an example of a direct-current / far-infrared ceramic heater used in the heat treatment apparatus.
  • Fig. 3 is a perspective view showing another direct current / far infrared ceramic heater.
  • FIG. 4 is a plan view showing a state in which a raw drum tube of a photosensitive drum as a heat treatment object is concentrically housed in the direct current / far infrared ceramic heater of FIG.
  • FIG. 5 is a perspective view showing another direct current / far infrared ceramic heater.
  • FIG. 6 is a plan view showing the heating state of the raw tube by the far-infrared ceramic heater shown in FIG. 5;
  • FIG. 7 is a perspective view showing still another direct current / far infrared ceramic heater.
  • Fig. 8 is a plan view showing the heating condition of the raw tube by the far-infrared ceramic heater of Fig. 7;
  • FIG. 9 is a cross-sectional view showing a portion of the heat treatment apparatus of FIG. 1 in which the direct current / far infrared ceramic heater is attached to the elevating device.
  • FIG. 10 is a sectional view showing a structure of a pallet for holding a raw tube in the heat treatment apparatus of FIG. 1,
  • FIG. 11 is a front view showing the structure of another heat treatment apparatus according to the present invention
  • FIGS. 12 and 13 show the heat insulating material used in the heat treatment apparatus shown in FIG.
  • FIG. 14 is a front view showing the structure of still another heat treatment apparatus according to the present invention.
  • Fig. 15 shows the heat insulating material used in the heat treatment apparatus shown in Fig. 14 above.
  • FIG. 16 is a front view showing the configuration of still another heat treatment apparatus according to the present invention.
  • FIG. 17 is a plan view showing the relationship between the transfer rail, the pallet, and the direct current / far-infrared ceramic heater in the heat treatment apparatus shown in FIG.
  • FIG. 18 and FIG. 19 are graphs each showing an example of a temperature rise pattern in the method for drying a functional thin film of the present invention.
  • FIG. 20 is a circuit diagram showing an example of a control device for controlling the direct-current / far-infrared ceramics heater for implementing the method of drying the photosensitive drum of the present invention
  • FIG. 21 is a plan view showing an example of a conventional heat treatment apparatus
  • FIG. 22 is a front view of the above device.
  • the heat treatment apparatus shown in the figure has a plurality of raw pipes P,
  • a cylindrical direct-current / far-infrared ceramic heater movably arranged up and down with respect to the transport path P
  • the direct-current / far-infrared ceramic heater 1 heats the pipe P concentrically and heats it from the surroundings as shown by the two-dot chain line in the lower state, and the solid line in the figure in the upper state. Indicated by Thus, it is stored in the cooling means 4 and cooled.
  • the cylindrical direct-current / far-infrared ceramic heater 1 is not limited to a tube integrally formed of a conductive ceramic material, as shown in FIG.
  • a plurality of plate-shaped ceramic heaters 1 a, 1 a... Arranged in a cylindrical shape having a polygonal cross section (octagon in the figure) can also be used. .
  • the product name “INFRALEX-BIRRC” manufactured by Asahi Glass Co., Ltd. is marketed.
  • This material is obtained by sintering a mixture of a ceramic material and a metal material to form a conductive ceramic cylinder 10 or a ceramic body 12 and, at the same time, form a cylindrical body 10.
  • a metal material such as aluminum is laminated in a strip shape on the outer periphery of both ends or on both ends of the plate body 12 by a thermal spraying method, various vapor phase methods, a wet plating method, etc. 1 1, 1 3, 13 are formed.
  • 2.5 to 25 from the outer circumference 10 a and inner circumference 10 b of the cylindrical body 10 or the outer surface of the plate 12 It radiates the far-infrared rays to heat the object to be heat-treated (base tube 1).
  • the direct-current / far-infrared ceramic heater is a uniform heating element having a cylindrical body 10 or a body 12 itself having electrical conductivity. —Between the pair of electrodes 11 1 and 11 1 When a voltage is applied between the electrodes 13 and 13, the portions other than the both ends where the electrodes are formed generate heat evenly and evenly. The surface of the raw pipe P can be heated evenly. Further, since the direct current / far infrared ceramic heater 1 has good responsiveness to the applied power, there is an advantage that the heating rate and the like can be finely controlled as described later.
  • Heat transfer conductivity rate 4. 2 x 1 0- 3 calZ ° C ⁇ Sec ⁇ cm bending strength index: 5. 2 kg / mm 2
  • Direct energization * The radial distance between the inner peripheral surface 1 ⁇ b of the far-infrared ceramic heater 1 and the outer peripheral surface of the raw pipe P is not particularly limited, but is 5 to 300 mm. ⁇ : L is preferably within the range of 0 ma. Direct energization * Far-infrared ceramics If the radial distance between the inner peripheral surface 1 Ob of the heater 1 and the outer peripheral surface of the pipe P is less than 5 ram, the distance is too short and direct energization * Far-infrared If the ceramic heater 1 has a very small amount of non-uniform heat generation, it directly affects the drying state of the coating film of the pipe P, and the coating film becomes unevenly dried.
  • the direct-current / far-infrared ceramic ceramics 1 in FIGS. 3 and 4 are composed of a substantially homogeneous body 12 made of a conductive ceramic material, It is constituted by arranging a plurality of plate-shaped ceramic heaters 1 a, 1 a,... Having a pair of electrodes 13, 13 provided at both end portions in a polygonal cross section. I have.
  • the plate-shaped ceramic heaters 1a, 1a ... are arranged in a tubular shape with gaps g, g ... as shown in the figure to prevent current leakage. These gaps g, g ... can be used without clogging for efficient removal of the solvent vapor generated from the coating film as described above. In consideration of the operation, it is preferable to close the space with an insulating material such as rubber or a heat insulating material described later.
  • the number of polygons is not particularly limited.
  • the number of corners is preferably 6 or more. If the number of corners of the polygon is 5 or less, the difference in the radial distance between the apex of the polygon and the center of the side with respect to the outer peripheral surface of the cylinder or cylinder becomes large, and uniform heating is achieved. It may not be possible.
  • each plate ceramic heater 1 a Since it is easier to manufacture than a cylinder and can be formed thinner, the direct current, far-infrared ceramic heater 1 can be manufactured at low cost and light weight. I Therefore, the means for raising and lowering the direct-current / far-infrared ceramic heater 1 with respect to the transport path of the pipe P (elevating device to be described later) and the like can be simplified. There are advantages such as that the entire device can be manufactured at low cost.
  • the direct energization ⁇ far-infrared ceramic heater 1 and pipe P And can be relatively rotated during heating.
  • the rotation speed of the direct-current / far-infrared ceramic heater 1 or the pipe P is not particularly limited, but is preferably in the range of 5 to 4 ° r.p.m. If the rotation speed is less than 5 r.p.m., heating may be uneven, and if it exceeds 40 r.p.Di., wind generated by rotation may affect the coating film. In addition, it may be difficult to maintain high-speed rotation control.
  • the width of a and the gap g, and the distance between the plate-shaped ceramic heater 1a and the surface of the pipe P as the object to be heat-treated are determined by the diameter of the pipe, direct energization
  • a preferred numerical value can be appropriately selected according to the number of angles of the mixer 11 and the like.
  • a plate-shaped ceramic heater is used.
  • the plate-shaped ceramic heaters 1a, 1a, 1a and 1 are arranged so that the shortest distance (indicated by d in FIG. 4) between the inner wall surface of 1a and the outer peripheral surface of the shell P is 5 or more. It is preferable that 3 to be arranged in an octagon with a width 1 or more of the gap 2, g ...
  • the plate-shaped ceramic heater 1a has a very small amount of non-uniform heat generation, it directly affects the drying state of the coating film of the raw pipe P, and the coating film becomes non-uniform.
  • the vapor density of the solvent evaporated from the coating film becomes higher, as will be described later, direct energization ⁇
  • the solvent The steam flow may cause defects such as longitudinal stripes on the surface of the coating film.
  • the width of the gap g is less than 11M, current leakage may occur between the adjacent plate-shaped ceramics 1a and 1a.
  • the outer diameter of the tube P is smaller than the inner diameter of
  • the rod-shaped direct-current / far-infrared ceramic heater 9 may be arranged concentrically with the direct-current / far-infrared ceramic heater 1. As shown in FIG. 6 or 8, the direct current / far infrared ceramic heater 9 has a tube P directly housed in a cylindrical direct current * far infrared ceramic heater 11.
  • the tubular or rod-shaped direct-current / far-infrared ceramic heater 9 is preferably used because it has a small outer diameter of the above-mentioned INFRALEX-BIRRC.
  • At least one of the above-mentioned direct-current / far-infrared ceramic heaters 1 and 9 has a cylindrical direct-current / far-infrared ceramic facing the surface of the coated tube P on which the coating film is formed.
  • a wavelength filter may be interposed, which allows only the light to pass through and transmits other components.
  • the wavelength cut filter is generally selected from ND filters (Neutral Density Filters) used for wavelength selection in the far infrared region according to the thickness of the coating film. Wavelength transmitting force ⁇ , used as appropriate.
  • the wavelength region of far infrared rays to be transmitted by the above wavelength cut filter differs depending on the thickness of the coating film, for example, when the thickness of the coating film is about 5 to 4 OjMi.
  • the specific wavelength region is in the range of 25 to 1 ° 0.
  • Each of the direct-current and far-infrared ceramic heaters 1 described above is attached to the mounting seat 51 at the end of the lifting bar 5 of the lifting device as shown in FIGS.
  • the heat treatment apparatus shown in FIG. 1 is disposed so as to be able to move up and down with respect to the transport path of the raw pipe P.
  • air blow pipes 6 and 6 of the air blowing means are connected to the mounting seat 51.
  • the blower blows the drying air from the upper end to the lower end of the pipe P, and the solvent evaporated from the coating film is directly energized and far-infrared ceramic. Used to prevent stagnation in the night and dry the coating film efficiently.
  • the flow velocity of the drying air is preferably in the range of 0.01 to 3 m / sec, particularly 0.1 to 2 mZ seconds. If the flow rate of the drying air is less than 1.01 1 / sec, the solvent evaporated from the coating film cannot be sufficiently prevented from directly staying in the far-infrared ceramics. On the other hand, when the flow velocity of the drying air exceeds 3 mZ seconds, the temperature of the direct-current / far-infrared ceramic heater itself decreases, and the radiation efficiency may decrease.
  • the drying air When the drying air is turbulent, the coating film tends to be uneven.
  • a temperature difference occurs between the lower end and the upper end of the raw pipe P, and drying tends to be uneven. Therefore, the drying air flows down from the upper end of the pipe P to the lower end. It is preferable to be one.
  • the pallet 3 conveyed along the conveyance path on the conveyance rail 2 has a fitting groove 31 a into which the lower end of the base tube P is fitted.
  • the cylindrical convex part 31 for holding P in an upright state and the lower end of the direct-current and far-infrared ceramic heater 1 descending on the transport path are fitted to each other to Directly energized and far-infrared ceramics Provided with a fitting recess 32 for holding the heater 1 concentrically o
  • a non-heating area (lower end) corresponding to the electrode at the lower end of the direct-current / far-infrared ceramic heater 1 In order to keep the pipe ⁇ away from the area indicated by ⁇ in the figure, a step indicated by ⁇ in the figure is provided.
  • the direct current / far-infrared ceramic mixer is equipped with a blowing means for flowing dry air from the upper end to the lower end of the raw pipe ⁇ .
  • a blowing means for flowing dry air from the upper end to the lower end of the raw pipe ⁇ .
  • the cooling means 4 provided is directly energized after the heating of the base tube ⁇ and the far-infrared ceramics heater is overheated. As shown in Fig. 1, it is directly energized.
  • the cylindrical body 41 that houses the far-infrared ceramic heater 1 and the lower end opening of this cylindrical body Doors to close the door.
  • the plurality of heat insulating materials 7 surrounding the heater 11 are directly energized when the raw tube P is heated, and the far-infrared ceramic heater 11 is energized.
  • the difference from the heat treatment apparatus shown in FIG. 1 is that the heat treatment apparatus shown in FIG.
  • the other parts are the same as the previous device. That is, in the heat treatment apparatus shown in the figure, a plurality of pallets 3, 3,... Which are transported on the transport rail 2 while holding the raw pipe P in an upright state, and a transport path of the raw pipe P by the pallets 3, 3,. It is arranged to be able to move up and down, and in the descending state, the tube P is concentrically accommodated and is directly energized in a cylindrical shape to heat it from the surroundings.
  • Direct power supply • Cooling means 4 for housing and cooling the far-infrared ceramic heater 11 inside.
  • Insulation materials 7, 7... are directly energized. ⁇ It is used to confine the heat of the far-infrared ceramic heater 1 and heat the pipe P more efficiently. As shown in the figure, a cylindrical body having an inner diameter matching the outer circumference of the above-mentioned direct current / far infrared ceramic heater 1 is divided along the axial direction (four in the figure). The whole of the heat insulating materials 7, 7,... Is formed of a heat resistant heat insulating material, for example, a fiber having a diameter of about 3 ram made of mica and a ceramic material.
  • the heat insulating materials 7, 7,... are directly energized.
  • the heat-insulating materials 7 are tightly attached to the outer periphery of the directly energized, far-infrared ceramics heater 11 ( (See Fig. 12) Direct heating after heating of P is completed.
  • far-infrared ceramic heater 11 is cooled by cooling means 4, it is not directly interrupted and cooling of far-infrared ceramic heater 11 is not hindered. However, it is separated from the directly energized and far infrared ceramic heater 1 and cooled independently (see Fig. 13).
  • Cooling means 8 for independently cooling the heat insulating material 7, 7 ... separated from the far-infrared ceramic heater 1 is arranged below the transport rail 2 as shown in Fig. 11. Cooling air is supplied from a blowing means (not shown) to cool the heat insulating materials 7, 7,.
  • cooling means as shown by a dashed line in the figure, a cooling medium such as cooling water is circulated through each heat insulating material 7 to cool the heat insulating material 7,
  • a cooling tube 81 may also be used.
  • the cooling pipe 81 is made of polytetrafluoroethylene (Teflon, heat-resistant temperature of 260 ° C or less), silicone resin (heat-resistant temperature of 260 ° C or less), fluorine rubber (heat-resistant temperature) 3 ⁇ ⁇ ° C or less).
  • the cylindrical direct-current * far-infrared ceramic heater 1 is a cylindrical heater made up of the eight rectangular ceramic heaters 1a, 1a, etc. described above. During cooling, these plate-shaped ceramic heaters la, la ... are separated into four blocks 1b, 1b ..., two by two, as shown in Fig. 15. The point that each of them is separately cooled in the main body 41 of the cooling means 4 is a difference from the above two devices.
  • a tube-shaped direct current supply for concentrically housing the pipe P and heating from the surroundings ⁇ Far-infrared ray ceramic heater 1 and a direct current rise from the transport path
  • Cooling means 4 for containing and cooling the mix heater 1 inside, and direct energization assembled into a cylindrical shape when heating the pipe P * Surrounds the far-infrared ceramic heater 1 And a plurality of heat insulating materials 7, 7.
  • each block 1b, 1b ... is divided into four parts, and then, as shown by the black arrows in FIG. b, 1 b-, and are independently cooled in cooling means 8 arranged below the transport rail.
  • This heat treatment apparatus is provided with two sets of upper and lower transfer rails 2a and 2b for alternately transferring a plurality of raw pipes P 1 and P 2, and sandwiches the two sets of transfer rails 2 a and 2 b.
  • the difference from the above three devices is that two sets of cylindrical direct-current and far-infrared infrared ceramic heaters 1A and 1B are provided.
  • the dried tube P is directly energized by moving the pallet 3a.Two sets of tubes are carried out. ⁇ The unheated tube is taken out from between the far-infrared ceramic heaters 1A and 1B. The upper pallet 3b holding P moves to enter between the above two sets of cylindrical direct energized * far-infrared ceramic heaters 1A and 1B.
  • the far-infrared ceramic heater 1 B rises as much as possible, and accommodates the pipe P held on the pallet 3 b concentrically and heat-drys the coating film. Do.
  • the transfer rails 2a and 2b have a gauge G wider than the outer diameter of the direct current / far infrared ceramic heaters 1A and IB. Is formed. Therefore, the movement of the direct-current / far-infrared ceramic heaters 1A and IB moving up and down across the transfer rails 2a and 2b is not hindered by the transfer rails 2a and 2b.
  • the heat treatment apparatus shown in the figure above while the tube P is being dried by one of the direct current and far infrared ceramic heaters, the other direct current can be cooled by the far infrared ceramic heater. Therefore, there is an advantage that the waiting time for direct energization and cooling of the far infrared ceramic heater can be omitted, and the photosensitive drum can be dried more efficiently.
  • a direct current / far-infrared ceramic once cooled by the cooling means 4 is used.
  • the direct current and far-infrared ceramic heater 1 are energized to generate heat, and the temperature of the tube P rises from room temperature to a predetermined heating temperature.
  • a method of heating for a predetermined time and drying the coating film of the polymer-based coating liquid formed on the surface of the base tube P is adopted.
  • the far-infrared ceramic heater 1 is temporarily cooled by the cooling means 4 only when the heating of the tube P is completed. This is to prevent the coating film from being rapidly heated by being covered with the next raw pipe P in the state.
  • the coating film formed by applying a high molecular weight coating solution to the surface of the base tube P is subjected to predetermined natural drying. * Direct drying * Far-infrared ceramic heater 1 drying power
  • the temperature rise of the raw tube P by the direct current / far-infrared ceramic heater depends on the composition and blending amount in the polymer coating solution as shown in FIG. 18 or FIG.
  • Tg glass transition temperature
  • the heating pattern shown in Fig. 18 is based on the glass transition temperature of the coating film. Until the middle I point, the temperature of the pipe P is rapidly increased, and after the glass transition temperature, the heating rate is reduced, and the temperature is gradually increased to the predetermined heating temperature, and reaches the predetermined heating temperature ( The temperature rise is stopped at the point ⁇ in the figure), and the above temperature is maintained until the drying is completed. Note that the same heating rate may be maintained between the point I and the point ⁇ as shown by a solid line in the same figure, and a point of inflection ( Through the two inflection points (points I-a and I-b in the figure), control may be performed so that the heating rate decreases gradually. Although not shown, a curve may be provided between the point I and the point ⁇ ⁇ .
  • the heating pattern shown in Fig. 19 indicates that the temperature of the pipe P rises rapidly until the glass transition temperature of the coating film (point ⁇ in the figure), and the glass transition temperature takes a specified time (see Fig. 19). (Up to the middle W point.) After the heating is stopped, the temperature is raised again. When the specified heating temperature is reached (point V in the figure), the heating is stopped again and until the drying is completed. The above temperature is maintained.
  • a control device for controlling the heating of the pipe P by the direct current and far-infrared ceramic heater 1 stepwise as in the above two examples for example, the configuration shown in Fig. 20 is adopted. Is done.
  • the control device shown in the figure is directly energized from the power supply ⁇
  • the SCR unit U2 that controls the drive power supplied to the far-infrared ceramic heater 1 based on the instruction from the temperature control unit U1,
  • An inverter U3 for controlling the drive of a fan F for supplying drying air to the far-infrared ceramic heater 1,
  • a sequencer U4 for controlling the temperature control means U1 and the inverter 3 It has.
  • the sequencer U 4 is directly energized.
  • the procedure for controlling the temperature of the pipe ⁇ ⁇ ⁇ by the far-infrared ceramic heater 1, the timing for rotating the fan F, and the glass transition temperature of the polymer material in the coating film And the like are stored as data, and based on this data, the temperature control means U1 and the member overnight U3 are controlled.
  • the temperature control means U 1 includes a sequencer U 4 By controlling the SCR unit U2 based on these instructions to adjust the power supplied to the direct energization * far-infrared ceramic heater 1, the direct energization * far-infrared ceramic heater 1
  • a temperature sensor C for measuring the temperature of the raw pipe P is connected when the heating of the raw pipe P is controlled step by step.
  • the temperature control means ⁇ 1 and the inverter U3 are output from the sequencer U4 based on data stored in advance. Then, a sequential control signal is sent. Then, the temperature control means U 1, which receives the control signal from the sequencer U 4, controls the SCR unit U 2 while measuring the temperature of the base tube ⁇ ⁇ ⁇ ⁇ with the temperature sensor C, and directly energizes * Far-infrared cell
  • the heating temperature of the raw tube ⁇ ⁇ ⁇ by the mixer 11 is controlled stepwise as shown in, for example, FIG. 18 or FIG. 19 described above, and the control signal is received from the sequencer U4.
  • the member U3 drives the fan F according to the procedure to dry the pipe ⁇ .
  • the heat treatment apparatus of the present invention is configured as described above, and heats the object to be heat-treated concentrically in a cylindrical direct-current / far-infrared ceramic heater.
  • the object to be heat-treated can be uniformly heat-treated.
  • the space cost for installation, heat treatment time, energy consumption, and the like can be greatly reduced.
  • the method for drying a functional thin film of the present invention after the glass transition temperature of the coating film, a force for slowly raising the temperature or temporarily stopping the heating, the above-mentioned coating film is formed.
  • the coating film can be evenly dried to the inside without defects such as fuse skin, air bubbles, pinholes, and repelling. It is possible to form a uniform functional thin film with small stress.
  • the heat treatment apparatus and the method for drying a functional thin film of the present invention are not limited to the above examples.
  • the direct energization * far-infrared ray ceramic heater is moved up and down with respect to the transport path of the tube P.
  • the tube P may be moved up and down.
  • the pallet 3, the transfer rail 2, the cooling means 4, the elevating bar 5 of the elevating device, the blower pipe 6 of the blowing means, and the heat insulation are provided to further efficiently dry the raw pipe P.
  • the material 7 and the cooling means 8 were provided, these members are not necessarily required for the present invention, and at least a cylindrical direct-current / far-infrared ceramic mixer is required. If provided, other configurations are not particularly limited.
  • each of the above heat treatment apparatuses has been used for drying a photosensitive layer of a photoreceptor drum as a functional thin film.
  • the heat treatment apparatus of the present invention has other functionalities as described above. It can be used for other purposes such as the formation of thin films, annealing of tacky or vapor-deposited films formed on the surface of substrates, sintering of ceramics formed into columns or tubes, and quenching of metals. Can be.
  • the object to be heat treated is a cylindrical photoreceptor drum, it is used as a direct-current / far-infrared ceramic heater, and has a cylindrical shape or a polygonal cross section having 6 or more corners.
  • a cylindrical shape was used, when it is used for heat-treating a heat-treated object having a different cross-sectional shape, an appropriate cross-sectional shape that is optimal for uniformly heating the heat-treated object is used. It is sufficient to use a cylindrical direct energizing and far-infrared ceramic mixer.
  • the temperature control after reaching a predetermined heating temperature is not particularly limited, and for example, temperature control such as gradually lowering the temperature is possible.
  • the method for drying a functional thin film of the present invention includes the steps of:
  • the present invention can be applied to drying of a functional thin film other than the photosensitive layer, such as a heat-generating coating film made of a heat-generating paint in which a heat-generating element is dispersed.
  • the following components were mixed and dispersed using an ultrasonic disperser to prepare a polymer coating solution for a single-layer photosensitive layer.
  • N, N'-di (3,5-dimethylphenyl) perylene 3,4,9,10-tetracarbodiimide 5 parts by weight
  • Tetrahydrofuran predetermined amount
  • the above polymer coating solution was immersed and applied to the surface of an aluminum tube with an outer diameter of 78 imn and a total length of 344, and allowed to air dry at room temperature (20 ° C) for 3 minutes to give a thickness of 2 mm. 2 A coating film of JM1 was formed.
  • the above-mentioned tube is 1975 mm in inside diameter, and the total length of 450 is recommended, and it is a direct cylindrical power supply without any seam.
  • ⁇ It is concentrically housed in a far-infrared ceramic heater. From the room temperature (20 ° C), the glass transition of the coating film was observed according to the pattern in which the temperature from point I to point ⁇ was linearly drought as shown by the solid line in the figure. 30 seconds to temperature (62 ° C) To raise the temperature (point I in the figure), and then reduce the heating rate to
  • the temperature was raised to 100 ° C (point ⁇ in the figure). Thereafter, drying was performed for 10 minutes from the start of heating while maintaining the above-mentioned temperature of 100 ° C. to form a single-layer type photosensitive layer on the surface of the raw tube, thereby producing a photosensitive drum.
  • a photoreceptor drum was manufactured in the same manner as in Experimental Example 1 except that the coating film was dried by a direct-current far infrared ray ceramic heater in the following heating pattern.
  • a photosensitive drum was manufactured in the same manner as in Experimental Example 1 except that the coating film was dried with a far-infrared ceramic heater in the following heating pattern.
  • the temperature was raised from room temperature (20 ° C) to the glass transition temperature (62 ° C) of the coating film in 30 seconds (point ⁇ in the figure). Then, the heating was stopped, and the above value 62 was maintained until 330 seconds after the start of heating (point IV in the figure). Next, start heating again and heat Starting 3 9 0 seconds later allowed to warm to 1 0 0 ° C (Fig. In V point), then while maintaining the 1 0 ⁇ ° C, c experimental examples were dried for 10 minutes from the start of heating Four
  • Direct energization ⁇ As a far-infrared ceramic heater, a plate-shaped ceramic heater with a width of 70 ram and a total length of 450 ram (manufactured by Asahi Glass Co., Ltd., trade name: INFRALEX-BIRRC) 8 sheets Of octagonal cross section (d in Fig. 3 (b) is 47 mm) with a 2 mm gap closed by insulating rubber.
  • a photosensitive drum was produced in the same manner as in Experimental Example 1 except that drying was performed while rotating the infrared ceramic heater at a rotation speed of 20 r, pm relative to the infrared ceramic heater.
  • a photosensitive drum was produced in the same manner as in Experimental Example 4 except that the same heating pattern as in Experimental Example 2 was employed.
  • a photosensitive drum was manufactured in the same manner as in Experimental Example 4 except that the same heating pattern as in Experimental Example 3 was used.
  • a photoreceptor drum was produced in the same manner as in Experimental Example 1 except that the coating film was dried with a far-infrared ceramics heater using a heating pattern shown below.
  • the temperature was raised linearly from room temperature (at 2 ° C) to 100 ° C in 10 seconds, and then the drying was completed for 10 minutes from the start of heating while maintaining the temperature at 100 ° C.
  • Each of the photoreceptor drums was loaded into an electrostatic copying tester (Gentec Shinshio 30M, manufactured by Gintech), the surface thereof was charged positively, and the surface potential Vs.p. (V) was measured.
  • Each of the charged photosensitive drums is exposed using a halogen lamp, which is an exposure light source of the electrostatic copying test apparatus, and the time until the surface potential V sp (V) is reduced to half is determined. E 1/2 (AJ / cm 2 ) was calculated.
  • V V 2 sp (V)-V! sp (V)
  • the photosensitive drums obtained in Experimental Examples 1 to 6 all have better photosensitive characteristics than Experimental Examples 7 and 8, and have a higher density of the photosensitive layer on the surface of the raw tube.
  • the photosensitive layer of each experimental example was observed, air bubbles, pinholes, repelling, etc. were not observed at all in any case.
  • the layer was excellent without defects. From this fact, it was found that, in the above experimental examples 1 to 6, the coating film could be dried uniformly to the inside and + minutes, and a photosensitive layer having no defect and having uniform internal stress could be formed. did.
  • the amount of residual solvent in the coating film was measured by pyrolysis chromatography as needed. of between from ⁇ point to IV point, the residual solvent amount of the coating film 1 mg is reduced to 5 X 1 0- 3 ⁇ 1 ⁇ i? Z rag, then when rapidly heated, formed photosensitive It was found that the amount of residual solvent in the layer could be reduced to almost ⁇ .
  • the functional thin film is formed by drying the polymer-based coating solution applied to the surface of the columnar or cylindrical substrate. It is suitable for use in the formation of a film, annealing of a sticking film or a vapor-deposited film formed on the surface of a substrate, sintering of a ceramic formed into a column or a cylinder, quenching of a metal, and the like.
  • the method for drying a functional thin film according to the present invention can prevent the surface of the coating film from drying before the inside, and can evenly dry the coating film to the inside. It is suitable for drying functional thin films such as a photosensitive layer of a photoreceptor drum and a conductive heating film made of a conductive heating coating in which a heating element is dispersed in an organic matrix.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Microbiology (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Resistance Heating (AREA)
  • Drying Of Solid Materials (AREA)
  • Photoreceptors In Electrophotography (AREA)

Abstract

Dispositif de traitement thermique pourvu d'un élément chauffant céramique cylindrique à infrarouges extrêmes alimenté directement, servant à chauffer un objet cylindrique ou en forme de colonne destiné à être traité, qui est concentrique à l'élément chauffant qui l'entoure. Ce dispositif permet d'effectuer un traitement thermique uniforme d'un objet. On décrit également un procédé de séchage d'une pellicule de revêtement composée d'un liquide de revêtement polymère formée à la surface d'un substrat cylindrique ou en forme de colonne, grâce à une configuration chauffante spécifique obtenue par l'utilisation du dispositif de traitement thermique décrite. Ce procédé de séchage empêche que la surface de la pellicule de revêtement ne sèche avant la partie interne, de manière à obtenir un séchage uniforme également de la partie interne de la pellicule de revêtement.
PCT/JP1990/001535 1989-11-28 1990-11-26 Dispositif de traitement thermique et procede de sechage de pellicules minces fonctionnelles utilisant ledit dispositif WO1991008655A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1019910700785A KR920702179A (ko) 1989-11-28 1990-11-26 열처리장치 및 이것을 사용한 기능성 박막의 건조방법

Applications Claiming Priority (4)

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JP30838589 1989-11-28
JP1/308385 1989-11-28
JP2004824A JPH03233885A (ja) 1989-11-28 1990-01-12 熱処理装置およびこれを用いた機能性薄膜の乾燥方法
JP2/4824 1990-01-12

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WO1991008655A1 true WO1991008655A1 (fr) 1991-06-13

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EP (1) EP0456829A4 (fr)
JP (1) JPH03233885A (fr)
KR (1) KR920702179A (fr)
WO (1) WO1991008655A1 (fr)

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DE4336857A1 (de) * 1993-10-28 1995-05-04 Bayerische Motoren Werke Ag Verfahren zum Trocknen von Automobillacken
FR2869831B1 (fr) * 2004-05-06 2006-06-30 Heights France Sas Soc Par Act Procede de sechage-desorption de plaques de flexogravure par exposition a un rayonnement en l'absence de circulation d'air chaud, et enceinte de mise en oeuvre du procede
JP4180562B2 (ja) 2004-12-09 2008-11-12 シャープ株式会社 電子写真感光体の製造方法および塗膜の乾燥方法
JP4654131B2 (ja) * 2006-02-07 2011-03-16 株式会社リコー 表面層加熱処理装置、表面層加熱・急冷処理装置
JP4824495B2 (ja) * 2006-07-18 2011-11-30 株式会社リコー 連続加熱処理装置
DE102007060105A1 (de) * 2007-12-13 2009-06-18 Eisenmann Anlagenbau Gmbh & Co. Kg Vorrichtung zum Trocknen von Gegenständen, insbesondere lackierten Fahrzeugkarosserien
US9904186B2 (en) 2011-08-05 2018-02-27 Fuji Electric Co., Ltd. Electrophotographic photoreceptor, method for manufacturing same, and electrophotographic apparatus using same
JP6020679B2 (ja) * 2015-07-15 2016-11-02 富士電機株式会社 電子写真用感光体、その製造方法およびそれを用いた電子写真装置
DE102022124575A1 (de) * 2022-09-23 2024-03-28 Duo Technik Gmbh Vorrichtung zum Trocknen von Flächengebilden
US11840609B1 (en) * 2023-04-12 2023-12-12 King Faisal University Method to prepare superhydrophobic sheets from virgin and waste polypropylene

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JPS5216055U (fr) * 1975-07-23 1977-02-04
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JPS61203292U (fr) * 1985-06-07 1986-12-20
JPS62241286A (ja) * 1986-04-10 1987-10-21 真空理工株式会社 赤外線加熱炉
JPS6330360A (ja) * 1986-06-04 1988-02-09 工業技術院長 酸化第二鉄焼結体及びセラミツクス赤外線ヒ−タ
JPH01289087A (ja) * 1988-05-14 1989-11-21 Toho Rayon Co Ltd 繊維の加熱処理装置

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JPS5216055U (fr) * 1975-07-23 1977-02-04
JPS59123180A (ja) * 1982-12-24 1984-07-16 ソ−ン　イ−エムアイ　ドメスティック　アプライアンス　リミテッド 加熱装置
JPS61203292U (fr) * 1985-06-07 1986-12-20
JPS62241286A (ja) * 1986-04-10 1987-10-21 真空理工株式会社 赤外線加熱炉
JPS6330360A (ja) * 1986-06-04 1988-02-09 工業技術院長 酸化第二鉄焼結体及びセラミツクス赤外線ヒ−タ
JPH01289087A (ja) * 1988-05-14 1989-11-21 Toho Rayon Co Ltd 繊維の加熱処理装置

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Also Published As

Publication number Publication date
JPH03233885A (ja) 1991-10-17
EP0456829A1 (fr) 1991-11-21
EP0456829A4 (en) 1992-05-13
KR920702179A (ko) 1992-08-12

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