JP6562273B2 - Plasma processing apparatus and method - Google Patents

Description

  The present invention relates to a plasma processing apparatus and method. More specifically, the present invention relates to a plasma processing apparatus and a processing method thereof that are compact but greatly increase the processing amount per one processing object such as powder and have a short processing time.

  Plasma is used for thin film formation, surface treatment and surface modification, decomposition and detoxification of air pollutants. Among these, atmospheric pressure plasma generated under atmospheric pressure does not require a vacuum device like low-pressure plasma, and plasma treatment with atmospheric pressure plasma is a relatively inexpensive and industrially advantageous technique.

  On the other hand, for the purpose of modifying the surface of powder under atmospheric pressure, a technique relating to a powder surface treatment apparatus using atmospheric pressure plasma is known (for example, see Patent Document 1). In this technique, the surface of the powder is modified by applying a voltage between the upper and lower electrodes externally fitted to the glass tube while the powder is uniformly blown up in the glass tube by the gas passing through the filter. However, since powder is blown up only by gas pressure in a thin glass tube to separate individual powders, the amount of processing per one time (hereinafter simply referred to as “processing amount”) is small.

  Therefore, as a result of various studies, the inventor has obtained a thick bar-shaped center electrode, and a cylindrical peripheral electrode arranged concentrically through gaps partitioned into a plurality of rooms outside the center electrode. And forming a discharge vessel in which at least one of the facing surfaces of both electrodes is covered with a dielectric, and rotating the discharge vessel with an alternating current or pulse voltage applied between the electrodes, It has been found that the amount of body treatment can be increased (see Patent Document 2). According to this technology, the powder sealed in each room, which is the discharge area of the glow discharge, is efficiently stirred regardless of the gas pressure to ensure a good and uniform surface quality, and the radial direction of the void By increasing the size of the discharge vessel and increasing the amount of stored powder while maintaining the thickness at a predetermined thickness, the amount of processed powder could be increased.

  However, as industrialization of atmospheric pressure plasma treatment of powder progresses, the demand for further increase in processing amount has been increasing in recent years. Therefore, instead of the center electrode described above, it is possible to use an electrode having a structure in which the powder can freely flow in the discharge vessel, for example, a mesh electrode or a plurality of thin rod electrodes (see, for example, Patent Document 3). ). According to this, the discharge vessel is rotated, and the powder can freely flow between the center portion and the outer peripheral portion in the discharge vessel through the mesh of the mesh electrode and the gap between the adjacent thin rod electrodes. By efficiently stirring the powder to ensure a good and uniform surface quality, the powder is also stored in the center, and the storage amount is increased without changing the size of the discharge vessel. The amount of processing is expected to increase.

Japanese Examined Patent Publication No. 7-68382 Japanese Patent No. 5080701 JP 7-157302 A

  However, when examined in detail, in the above-described mesh electrode, when the surface of the mesh made of stainless steel wire or the like is coated with a dielectric such as glass, it is difficult to make the coating thickness of the dielectric uniform over the entire mesh. In particular, when a mesh is immersed and coated in a dielectric material such as molten glass, if the coating thickness due to the dielectric varies greatly between the intersections or straight portions of the mesh, or if the mesh is small, the mesh is caused by the dielectric. May be blocked. For this reason, the glow discharge generated from the mesh electrode becomes unstable, and local dielectric breakdown or peeling occurs, which easily damages the electrode. In addition, when the number of meshes closed by the dielectric is large, the amount of powder flowing between the central portion and the outer peripheral portion in the discharge vessel is reduced, and even efficient powder agitation becomes difficult.

  Further, in the above-mentioned Patent Document 3 relating to a plurality of thin rod-shaped electrodes, among a plurality of rod-shaped electrodes arranged in an annular shape (hereinafter referred to as a “rod-shaped electrode group”), In addition, since it is necessary to provide a discharge region, the inner diameter of the rod-shaped electrode group is limited to be small. For this reason, a large amount of powder cannot be stored in the center, and it is difficult to significantly increase the amount of stored powder.

  On the contrary, if the inner diameter of the rod-shaped electrode group is increased to increase the amount of powder stored in the center, the glow discharge inside the rod-shaped electrode group becomes unstable. Only outside. For this reason, unlike the case of Patent Document 2 in which plasma is continuously irradiated on the powder in a plurality of rooms, the powder can be irradiated only with plasma intermittently, and the processing time required for the plasma processing becomes longer.

  The present invention has been devised in view of the above points, and is a compact plasma processing apparatus that greatly increases the processing amount per time of an object to be processed such as powder and has a short processing time, and It aims at providing the processing method.

  In order to achieve the above object, the plasma processing apparatus of the present invention is provided with discharge rods formed by covering rod-shaped electrodes with a first dielectric material in a substantially annular shape at predetermined circumferential intervals substantially parallel to each other. An electrode unit disposed outside the electrode unit, the object to be processed is sealed inside, a cylindrical discharge container having a second dielectric, and an external electrode body disposed outside the discharge container A rotating device that rotates the discharge vessel in a state where glow discharge is generated by applying an alternating current or a pulse voltage between the electrode unit and the external electrode body, and a discharge area of the glow discharge is set between the inside and outside of the electrode unit. It has a discharge area expansion structure that can be expanded.

  Then, by forming the discharge rod by covering the rod-shaped electrode with the first dielectric, it is possible to reduce the component cost by improving the electrode life and to reduce the size of the power supply facility by reducing the load. That is, the rod-shaped electrode is covered with a first dielectric having a substantially constant thickness, and a stable glow discharge is generated, and local breakdown and peeling can be suppressed to prevent the discharge rod from being damaged. The electric field concentration effect facilitates the start of discharge and reduces the burden on the power supply.

  Furthermore, by providing an electrode unit in which the discharge rods are arranged substantially in parallel with each other at a predetermined circumferential interval, it is possible to ensure a good and uniform surface quality of the object to be processed and to cover the inside of the electrode unit. It is possible to store the processed material. In other words, the workpiece can flow freely between the inside and outside of the electrode unit through the gap between the discharge rods that are not likely to be blocked due to the stable glow discharge, thereby increasing the movement space of the workpiece. This ensures that the workpiece can be efficiently stirred, and the workpiece also flows inside the electrode unit.

  In particular, when each discharge rod is made separate and separable from each other, the maintainability of the electrode unit and the immediate response to the functional group change can be improved. In other words, when the discharge rod is damaged, it is only necessary to replace the damaged discharge rod, not the entire electrode unit, and when changing the functional group to be added to the object to be processed, the already disposed discharge It is sufficient to replace the rod with a discharge rod having a first dielectric containing a component capable of supplying a predetermined functional group at the time of discharge, mixing of the functional group-containing gas into the inert gas, No additional input of base feed is required.

  In addition, the cylindrical discharge vessel is disposed outside the electrode unit, the object to be processed is enclosed inside, and has a second dielectric, the external electrode body disposed outside the discharge vessel, and the electrode By providing a rotating device for rotating the discharge vessel in a state where glow discharge is generated by applying an alternating current or a pulse voltage between the unit and the external electrode body, a significant increase in the amount of processing of the object to be processed is achieved. Can be planned. In other words, during plasma treatment, all the discharge rods in the same electrode unit are set to the same potential, and the glow discharge is not generated between the discharge rods that are spaced apart from each other across the center, thereby expanding the inner diameter of the electrode unit. This makes it possible to greatly increase the amount of material to be processed. Moreover, the object to be processed enclosed in the discharge vessel freely flows between the inside and outside of the electrode unit through the gap between the discharge rods while the discharge vessel is rotated, and the stable discharge region is efficiently stirred. As a result, the surface of the object to be processed is uniformly processed, and a good and uniform surface quality can be ensured.

  Furthermore, by providing a discharge area expansion structure that can expand the discharge area of the glow discharge to the inside and outside of the electrode unit, the processing time of the plasma treatment can be greatly shortened. That is, by extending the discharge region, the time for the workpiece to pass through the discharge region is increased, and the plasma irradiation time can be increased.

  Further, in the discharge vessel, both the radial interval between the first dielectric and the second dielectric and the circumferential interval between adjacent first dielectrics in the discharge vessel are 2 to 20 mm. In this case, the gap from the glow discharge to the arc discharge due to the high voltage application is appropriately restricted while ensuring a sufficient gap around the discharge rod for the flow of the object to be processed. In addition, the circumferential interval is appropriately limited to optimize the overlap of the discharge areas of the glow discharge by the adjacent discharge rods. As a result, it is possible to secure a discharge region that can be processed for a short time with an appropriate plasma density under a stable glow discharge without hindering the flow of the workpiece.

  When the radial interval is less than 2 mm, the flow resistance when the workpiece passes through the gap between the first dielectric and the second dielectric is increased, and the flow of the workpiece in the discharge region is inhibited. Is done. On the other hand, when the radial interval exceeds 20 mm, the distance between the discharge rod and the external electrode body increases, and the voltage required for the discharge between both electrodes also increases. The glow discharge becomes unstable.

  Furthermore, when the circumferential interval is less than 2 mm, the flow resistance when the workpiece passes through the gap between the adjacent first dielectrics increases, and the flow of the workpiece between the inside and outside of the electrode unit is hindered. . On the other hand, if the interval in the circumferential direction exceeds 20 mm, the overlapping part of the glow discharge irradiated areas by the adjacent discharge rods becomes small, and the plasma density becomes insufficient.

  In addition, the discharge area expanding structure includes a sub-electrode unit in which the discharge rods are arranged in a substantially annular shape at a predetermined circumferential interval substantially parallel to each other in a space inside the electrode unit. When there is a single or a plurality of concentric electrodes, when an alternating current or pulse voltage is applied between the electrode unit and the sub-electrode unit, or between the sub-electrode units adjacent inside and outside, the glow discharge discharge area becomes inward of the electrode unit. Also formed. Thereby, the time for the workpiece to pass through the discharge region becomes longer, the plasma irradiation time can be lengthened, and the processing time of the plasma treatment can be greatly shortened.

  In the discharge vessel, the radially innermost sub-electrode unit is replaced with a predetermined discharge rod, and a cooling type discharge rod in which a cooling medium can flow in an internal gap between the rod-shaped electrode and the first dielectric, In the case where the cooling medium has at least one of the first dielectric simple substance capable of flowing inside, cooling is difficult by flowing the cooling medium through the internal gap of the cooling type discharge rod and the internal space of the first dielectric. The discharge rod at the center side of the discharge vessel can be efficiently cooled. As a result, it is possible to prevent objects to be processed such as resin flowing in the discharge vessel from being welded to each other due to heat accompanying discharge, adhering to the inside of the vessel, or changing the surface. It is possible to improve the quality of objects and to expand the application target of plasma treatment.

  Also, a cooling type discharge cylinder that is disposed on the axial center in the discharge vessel and is formed by covering a cylindrical electrode with a cooling medium that can flow through the inside with a third dielectric, or disposed on the axial center. When the cooling medium is provided with the third dielectric single body that can flow inside, the discharge is difficult to cool by flowing the cooling medium through the cylindrical electrode of the cooling type discharge cylinder or the internal space of the third dielectric. The discharge rod on the center side of the container can be efficiently cooled. As a result, it is possible to prevent objects to be processed such as resin flowing in the discharge vessel from being welded to each other, adhered to the inside of the vessel, or the surface from being altered by the heat accompanying the discharge. Therefore, it is possible to improve the quality of the object to be processed and to expand the application target of the plasma treatment.

  In addition, the discharge area expanding structure supports the discharge rod by attaching only the end portion of the discharge rod to the axial end surface in the discharge vessel, and is disposed on substantially the same circumference to form a substantially ring. A plurality of arcuate mounting members that can be formed, a radial support member in which a plurality of branch portions extend radially from the axis of the substantially annular ring, and a mounting position of the mounting member with respect to the branch portions is changed to change the diameter. When adjusting the radial position of the mounting member by the adjusting mechanism, the gap between the first dielectric and the second dielectric is increased, and the discharge area of the glow discharge is increased. Is extended outside the electrode unit. Thereby, the time for the workpiece to pass through the discharge region becomes longer, the plasma irradiation time can be lengthened, and the processing time of the plasma treatment can be greatly shortened.

  In particular, when the discharge rod is energized in a state where the end of the discharge rod is insulated and supported by the radial support member, the end of the discharge rod is supported by an insulating member that contacts a wide range of other components. In contrast, it is possible to minimize the leakage of current to the outside through the surface of each member, and the power cost can be reduced.

  Further, a rake member that rotates together with the discharge vessel and whose outer peripheral side in the centrifugal direction is curved in the rotational direction, and an inflow port on the inner peripheral side in the centrifugal direction on the front side in the rotational direction of the rake member, communicates with the inflow port. A retention chamber, and a discharge port that communicates with the retention chamber and is located on the outer peripheral side in the centrifugal direction from the retention chamber and has a smaller area than the inflow port. When a stirrer blade having a stay discharge part that gradually flows down toward the discharge region through the discharge port through the stay chamber is provided, the discharge is performed when the axis of the discharge vessel is in a substantially horizontal posture or an inclined posture. The object to be processed collected in the lower part of the container is further efficiently stirred by the rotating stirring blades, and part of the workpiece is scooped up by the scooping member and flows into the staying chamber from the inlet, and then the stirring blades are connected to the discharge container. one Rotating in during the rise to the upper position from the lower position, the object to be treated which has flowed in through the discharge region flows down gradually by through its own weight outlet. Thereby, the time for the workpiece to pass through the discharge region becomes longer, the plasma irradiation time can be lengthened, and the processing time of the plasma treatment can be further greatly shortened.

  Further, the sieving member is rotated together with the discharge vessel, the outer peripheral side in the centrifugal direction is curved in the rotational direction, and the sieve discharge part having the discharge hole in the rotational direction has a rake member with a hole disposed on the outer peripheral side in the centrifugal direction. When the stirring blade is provided, when the axial center of the discharge vessel is in a substantially horizontal posture or an inclined posture, the object to be processed collected in the lower portion of the discharge vessel is further efficiently stirred by the rotating stirring blade, and The part is scooped up by a scooping member with a hole, and while the stirring blade rotates together with the discharge vessel and rises from the lower position to the upper position, it gradually flows down through the discharge hole of the sieve discharge part by its own weight and moves through the discharge area. pass. Thereby, the time for the workpiece to pass through the discharge region becomes longer, the plasma irradiation time can be lengthened, and the processing time of the plasma treatment can be further greatly shortened.

  Further, the electrode unit, the lid unit that closes the opening of the discharge vessel and supports the electrode unit, and the discharge rod that is adjacent to the electrode unit are interposed, and the axial end is fixed to the lid unit. In the case where the stirring blade supported by being slidably contacted with the inner wall of the discharge vessel is provided with the electrode structure integrally incorporated, the stirring blade is slid on the inner wall of the discharge vessel. By simply inserting the electrode structure into the discharge vessel while moving, the discharge rod of the electrode unit incorporated in the electrode structure together with the stirring blade is also held at a predetermined radial position from the inner wall. As a result, the electrode unit can be supported at an appropriate position using the stirring blade, a complicated support structure for the electrode unit is not required, and the cost of parts can be reduced and the maintainability can be improved. .

  Furthermore, the lid unit incorporated in the electrode structure together with the stirring blade is also held at a predetermined position with respect to the discharge vessel. Thus, the lid unit can be quickly positioned with respect to the discharge vessel using the stirring blade, and the assembly time required for assembling the plasma processing apparatus is shortened.

  In addition, the electrode structure is held in the discharge vessel only through the stirring blades, and is configured as a separate body that can be separated from the discharge vessel. As a result, only the object to be processed remains in the discharge vessel simply by detaching the electrode structure after the plasma treatment, so that the object to be processed can be easily collected and attached in the discharge vessel. The kimono can be easily removed, and the processing time required for the entire plasma processing can be shortened and the maintainability can be further improved.

  In addition, when the lid unit is attached so as to be openable and closable in a hole formed in the lid body that closes the opening, and has a plug portion in which a current path and a ventilation path for glow discharge are integrated, The current path and the ventilation path for glow discharge can be concentrated on the plug portion constituting the electrode structure. As a result, the current path and the ventilation path can be easily and quickly incorporated into the plasma processing apparatus simultaneously with the insertion of the electrode structure, the time required for assembly of the plasma processing apparatus can be shortened, and the working efficiency can be improved. it can.

  Further, only the plug portion of the electrode structure can be detached from the lid, and the hole of the lid can be opened. As a result, the portion of the electrode structure excluding the plug portion (hereinafter referred to as the “basic structure portion”) is inserted into the discharge vessel, and the object to be processed is placed in the discharge vessel through the opened hole. Therefore, it becomes easy to supply an object to be processed before the plasma processing and to supply the object to be processed during the plasma processing.

  In particular, when supplying an object to be processed before plasma processing, if the electrode structure is inserted while the object to be processed is stored in the discharge vessel, the tip of the electrode structure is placed on the bottom surface of the discharge vessel. In such a case, the base structure portion is first inserted into the discharge vessel, and after the workpiece is poured into the discharge vessel through the hole of the lid, the plug portion is inserted. Install in the hole. Thereby, a to-be-processed object can be supplied in a discharge vessel, without making it interfere with an electrode structure.

  In order to achieve the above object, the plasma processing method of the present invention comprises a discharge rod formed by covering a rod-shaped electrode with a first dielectric material in a substantially annular shape at a predetermined circumferential interval substantially parallel to each other. The disposed electrode unit is disposed on the inner side, the outer electrode body is disposed on the outer side, and a cylindrical discharge vessel having a second dielectric is interposed between the electrode unit and the outer electrode body, Applying an alternating current or pulse voltage between the electrode unit and the external electrode body while rotating the discharge vessel with an inert gas atmosphere inside the sealing step of sealing the object to be processed in the discharge vessel with a rotating device A processing step of performing plasma processing by flowing the object to be processed in a discharge region of glow discharge expanded inside and outside of the electrode unit by generating a glow discharge.

  Then, by forming the discharge rod by covering the rod-shaped electrode with the first dielectric, it is possible to reduce the component cost by improving the electrode life and to reduce the size of the power supply facility by reducing the load. That is, the rod-shaped electrode is covered with a first dielectric having a substantially constant thickness, and a stable glow discharge is generated, and local breakdown and peeling can be suppressed to prevent the discharge rod from being damaged. The electric field concentration effect facilitates the start of discharge and reduces the burden on the power supply.

  Furthermore, the electrode unit in which the discharge rods are arranged substantially in parallel with each other at a predetermined circumferential interval to ensure a good and uniform surface quality of the object to be processed, and the object to be processed inside the electrode unit. Storage can be possible. In other words, the workpiece can flow freely between the inside and outside of the electrode unit through the gap between the discharge rods that are not likely to be blocked due to the stable glow discharge, thereby increasing the movement space of the workpiece. This ensures that the workpiece can be efficiently stirred, and the workpiece also flows inside the electrode unit.

  In particular, when each discharge rod is made separate and separable from each other, the maintainability of the electrode unit and the immediate response to the functional group change can be improved. In other words, when the discharge rod is damaged, it is only necessary to replace the damaged discharge rod, not the entire electrode unit, and when changing the functional group to be added to the object to be processed, the already disposed discharge It is sufficient to replace the rod with a discharge rod having a first dielectric containing a component capable of supplying a predetermined functional group at the time of discharge, mixing of the functional group-containing gas into the inert gas, No additional input of base feed is required.

  In addition, the electrode unit in which the discharge rods formed by covering the rod-shaped electrodes with the first dielectric material are arranged in a substantially annular shape at a predetermined circumferential interval substantially in parallel with each other, while the external electrode body is arranged By disposing a cylindrical discharge vessel having a second dielectric between the electrode unit and the external electrode body, and providing an encapsulation step of enclosing an object to be processed in the discharge vessel, The versatility of plasma treatment for different surface treatments and surface modifications is improved. In other words, a functional group supply source suitable for surface treatment or surface modification is contained in the first dielectric, or simply placed in the discharge vessel together with the object to be treated, so that the electrode unit and the external electrode body in the subsequent process Various functional groups can be added to the object to be processed by glow discharge between them.

  Furthermore, the discharge region is expanded by applying glow or alternating current or pulse voltage between the electrode unit and the external electrode body while rotating the discharge vessel with an inert gas atmosphere inside by a rotating device. By providing a treatment step for performing plasma treatment by flowing the treatment object in a discharge region of a glow discharge extended in and out of the electrode unit in the structure, a significant increase in the amount of treatment of the treatment object, The processing time can be greatly shortened.

  In other words, during plasma treatment, all the discharge rods in the same electrode unit are set to the same potential, and the glow discharge is not generated between the discharge rods that are spaced apart from each other across the center, thereby expanding the inner diameter of the electrode unit. This makes it possible to greatly increase the amount of material to be processed. Moreover, the object to be processed sealed in the discharge vessel freely flows between the inside and outside of the electrode unit through the gap between the discharge rods while the discharge vessel is rotated, and the electrode unit and the external electrode body It passes through the stable discharge zone in between while being efficiently stirred, and the surface of the object to be processed is treated uniformly, and a good and uniform surface quality can be ensured. And by extending a discharge area, the time for a to-be-processed object to pass a discharge area becomes long, and a plasma irradiation time can be lengthened.

  Further, in the discharge vessel, both the radial interval between the first dielectric and the second dielectric and the circumferential interval between adjacent first dielectrics in the discharge vessel are 2 to 20 mm. In this case, the gap from the glow discharge to the arc discharge due to the high voltage application is appropriately restricted while ensuring a sufficient gap around the discharge rod for the flow of the object to be processed. In addition, the circumferential interval is appropriately limited to optimize the overlap of the discharge areas of the glow discharge by the adjacent discharge rods. As a result, it is possible to secure a discharge region that can be processed for a short time with an appropriate plasma density under a stable glow discharge without hindering the flow of the workpiece.

  When the radial interval is less than 2 mm, the flow resistance when the workpiece passes through the gap between the first dielectric and the second dielectric is increased, and the flow of the workpiece in the discharge region is inhibited. Is done. On the other hand, when the radial interval exceeds 20 mm, the distance between the discharge rod and the external electrode body increases, and the voltage required for the discharge between both electrodes also increases. The glow discharge becomes unstable.

  Furthermore, when the circumferential interval is less than 2 mm, the flow resistance when the workpiece passes through the gap between the adjacent first dielectrics increases, and the flow of the workpiece between the inside and outside of the electrode unit is hindered. . On the other hand, if the circumferential interval exceeds 20 mm, the overlapping part of the discharge areas of the glow discharge by the adjacent discharge rods becomes small, the plasma density becomes insufficient, and the processing time of the plasma processing becomes long.

  In addition, the discharge area expanding structure includes a sub-electrode unit in which the discharge rods are arranged in a substantially annular shape at a predetermined circumferential interval substantially parallel to each other in a space inside the electrode unit. When there is a single or a plurality of concentric electrodes, when an alternating current or pulse voltage is applied between the electrode unit and the sub-electrode unit, or between the sub-electrode units adjacent inside and outside, the glow discharge discharge area becomes inward of the electrode unit. Also formed. Thereby, the time for the workpiece to pass through the discharge region becomes longer, the plasma irradiation time can be lengthened, and the processing time of the plasma treatment can be greatly shortened.

  In the discharge vessel, the radially innermost sub-electrode unit is replaced with a predetermined discharge rod, and a cooling type discharge rod in which a cooling medium can flow in an internal gap between the rod-shaped electrode and the first dielectric, In the case where the cooling medium has at least one of the first dielectric single body capable of flowing inside, it is difficult to cool by flowing the cooling medium in the internal gap of the cooling type discharge rod, the internal space of the first dielectric. The discharge rod at the discharge vessel center side can be efficiently cooled. As a result, it is possible to prevent objects to be processed such as resin flowing in the discharge vessel from being welded to each other due to heat accompanying discharge, adhering to the inside of the vessel, or changing the surface. It is possible to improve the quality of objects and to expand the application target of plasma treatment.

  Also, a cooling type discharge cylinder that is disposed on the axial center in the discharge vessel and is formed by covering a cylindrical electrode with a cooling medium that can flow through the inside with a third dielectric, or disposed on the axial center. In the case where the cooling medium includes the third dielectric single body that can flow inside, it is difficult to cool the cooling medium by flowing the cooling medium in the cylindrical electrode of the cooling type discharge cylinder or the internal space of the third dielectric. The discharge rod at the discharge vessel center side can be efficiently cooled. As a result, it is possible to prevent objects to be processed such as resin flowing in the discharge vessel from being welded to each other due to heat accompanying discharge, adhering to the inside of the vessel, or changing the surface. It is possible to improve the quality of objects and to expand the application target of plasma treatment.

  In addition, the discharge area expanding structure supports the discharge rod by attaching only the end portion of the discharge rod to the axial end surface in the discharge vessel, and is disposed on substantially the same circumference to form a substantially ring. A plurality of arcuate mounting members that can be formed, a radial support member in which a plurality of branch portions extend radially from the axis of the substantially annular ring, and a mounting position of the mounting member with respect to the branch portions is changed to change the diameter. When adjusting the radial position of the mounting member by the adjusting mechanism, the gap between the first dielectric and the second dielectric is increased, and the discharge area of the glow discharge is increased. Is extended outside the electrode unit. Thereby, the time for the workpiece to pass through the discharge region becomes longer, the plasma irradiation time can be lengthened, and the processing time of the plasma treatment can be greatly shortened.

  In particular, when the discharge rod is energized in a state where the end of the discharge rod is insulated and supported by the radial support member, the end of the discharge rod is supported by an insulating member that contacts a wide range of other components. In contrast, it is possible to minimize the leakage of current to the outside through the surface of each member, and the power cost can be reduced.

  Although the plasma apparatus and method according to the present invention are compact, the processing amount per processing object such as powder is greatly increased, and the processing time is short.

It is a perspective view which shows the whole structure of the plasma processing apparatus concerning this invention. It is side surface sectional drawing similarly. FIG. 4 is a side cross-sectional view of the vicinity of a mounting portion of the discharge rods 6 and 26. It is AA arrow sectional drawing of FIG. FIG. 5A is an enlarged front sectional view of the sub-electrode unit, FIG. 5A is an enlarged front sectional view of the sub-electrode unit 21A, and FIG. 5B is an enlarged front sectional view of the sub-electrode unit 21B. FIG. 6A is a front sectional view of a plasma processing apparatus according to another embodiment, FIG. 6A is a front sectional view of the plasma processing apparatus 1A, and FIG. 6B is a front sectional view of the plasma processing apparatus 1B. It is a front view of plasma processing apparatus 1C of another form. It is explanatory drawing of the stirring blade of another form, Comprising: Fig.8 (a) is a perspective view of the stirring blade 60, FIG.8 (b) is front sectional drawing similarly. It is explanatory drawing of the stirring blade of another form, Comprising: Fig.9 (a) is a perspective view of the stirring blade 61, FIG.9 (b) is front sectional drawing similarly. It is a perspective view which shows the whole structure of plasma processing apparatus 1D of another form. It is side surface sectional drawing of plasma processing apparatus 1D of another form. FIG. 6 is a side cross-sectional view of the vicinity of the attachment portion of the discharge rod 6. 3 is a perspective view of a support structure 71. FIG. It is BB arrow sectional drawing of FIG. It is CC sectional view taken on the line of FIG. FIG. 10 is a front view of the vicinity of an adjustment mechanism 85. It is side surface sectional drawing of the plasma processing apparatus 1E of another form. It is side surface sectional drawing of a support block outer peripheral part. It is explanatory drawing of a decomposition | disassembly procedure. It is side surface sectional drawing of the plasma processing apparatus 1F of another form. It is also a front view. It is DD sectional view taken on the line of FIG. It is EE arrow sectional drawing of FIG. It is side surface sectional drawing of a cover unit periphery part. FIG. 25A is a side sectional view in the vicinity of the mounting portion of the discharge rod 6A, and FIG. 25B is a side sectional view in the vicinity of the mounting portion of the conductive bolt. It is explanatory drawing at the time of inserting a foundation structure part in a discharge vessel. It is explanatory drawing at the time of supplying powder through the hole of a foundation structure part. It is explanatory drawing at the time of detaching | desorbing an electrode structure from a discharge vessel. It is an expanded front sectional view of an electrode unit. It is a graph which shows the influence of the radial direction space | interval and circumferential direction space | interval which has on the discharge condition and fluidity | liquidity.

Hereinafter, embodiments of the present invention relating to a plasma processing apparatus and method thereof will be described with reference to the drawings for understanding of the present invention.
1, 10, and 17, the direction indicated by arrow F is the forward direction, the direction indicated by arrow L is the left direction, and the direction indicated by arrow T in FIG. 26 is the upward direction. The position, direction, etc. are based on these front, left, and upper directions.

  First, the overall configuration of the plasma processing apparatus 1 to which the present invention is applied will be described with reference to FIGS. 1 to 4 and 20.

  In the plasma processing apparatus 1, wheels 8L and 8R and wheels 9L and 9R are arranged on the front and back of the upper surface of the U-shaped base 7 in front view, and these wheels 8L, 8R, 9L and 9R are not shown. A rotating device 5 is formed which is linked to an output shaft from a rotating electric motor and can rotate the cylindrical discharge vessel 3 placed on the wheels 8L, 8R, 9L, 9R.

  Then, a strip-shaped anti-floating material 10 extends in the left-right direction so as to straddle between the left and right edge portions 7a, 7b of the base 7, and the right end of the anti-floating material 10 is The left end of the anti-floating material 10 is connected to the eaves member 11 erected from the left edge 7b of the base 7 through the long hole 10a. I can remove it. As a result, the entire levitation preventive material 10 is elastically surrounded by the outer periphery of the discharge vessel 3, and the discharge vessel 3 can be prevented from floating from the wheels 8L, 8R, 9L, 9R due to vertical vibrations or the like.

  In addition, the discharge vessel 3 described above includes a container body 12 having a bottomed cylindrical shape with a cup-shaped bottom 12b detachably attached to a rear end of the cylindrical body 12a by a fastener 38, and a front end of the body 12a. And a lid 13 for closing the opening 12a1 in an openable and closable manner.

  Among these, on the inner peripheral surface of the container main body 12, a long plate-like stirring blade 14 for scooping up the powder, which is an object to be processed, enclosed in the discharge container 3 in the circumferential direction, is used in this embodiment. It is attached via three leg portions 14a, 14b, and 14c provided in order from the front at approximately equal intervals in the circumferential direction.

  On the other hand, on the outer peripheral surface of the container main body 12, locking rings 15F and 15R whose front and rear outer surfaces are in contact with the front and rear inner surfaces of the wheels 8L, 8R, 9L and 9R described above are fitted to the front and rear. The locking rings 15F and 15R are fixed to the outer peripheral surface of the container main body 12 via stainless steel ring-shaped attachment bands 16F and 16R. Then, the locking rings 15F, 15R regulate the sliding of the discharge vessel 3 in the front-rear direction, and the discharge vessel 3 is prevented from sliding off from the wheels 8L, 8R, 9L, 9R due to the longitudinal vibration. Can do.

  Further, the lid 13 is detachably fixed to the opening 12a1 by a fixing tool 17 with a packing or the like (not shown) interposed between the opening 12a1 of the container body 12 and the like. As a result, the lid 13 is opened and the powder is poured into the container main body 12 from the opening 12 a 1, and then the lid 13 is closed again and fixed with the fixture 17, so that the powder is put inside the discharge vessel 3. Can be encapsulated.

  The lid 13 is integrally formed with a through cylinder 13a penetrating the shaft, and a sealing plug 18 usually made of rubber or the like is inserted into the through cylinder 13a. As will be described later, the sealing plug 18 can support the electrode unit 2 and the sub-electrode unit 21 and supply and discharge the mixed gas 37 containing helium gas, nitrogen gas and the like into the discharge vessel 3. ing.

  In addition, both the lid body 13 and the container body 12 described above are formed of glass as the second dielectric, and in the portion of the container body 12 where a later-described wire mesh 4 is externally fitted, Glow discharge by dielectric barrier discharge can be performed. In this embodiment, glass is used for the entire discharge vessel 3 so that the processing status during plasma processing can be observed from the outside. However, if there is no need for external observation, dielectrics such as plastic, ceramics, and aluminum oxide are used. A body may be used, and a material other than a dielectric may be used in addition to a portion where the wire mesh 4 is fitted.

  Further, on the outside of the container main body 12 of the discharge container 3, a stainless steel wire mesh 4 as an external electrode body is disposed between the above-described locking rings 15F and 15R.

  The attachment bands 16F and 16R described above are fitted on the front and rear edges of the wire mesh 4, and a part of the side surface of the wire mesh 4 is sandwiched between the front and rear ends of the attachment mesh 16F and 16R. The wire mesh 4 is fixed to the outer peripheral surface of the container body 12 so as to be held by a long plate-like attachment band 16S made of stainless steel.

  Further, the wire mesh 4 is grounded via the attachment bands 16F, 16R, 16S, and the ground wire 20 that connects the attachment bands 16F, 16S.

  In addition, the electrode unit 2 is disposed inside the container body 12 of the discharge container 3 in which the wire mesh 4 is disposed on the outside, and a discharge area expansion structure that will be described in detail later is provided in a space further inside the electrode unit 2. Are arranged concentrically.

  Of these, the electrode unit 2 is configured by arranging a plurality of discharge rods 6 in an annular shape in parallel with each other at a predetermined circumferential interval y. The discharge rod 6 is composed of a rod-shaped electrode 6a such as a stainless steel wire and a glass tube 6b surrounding the rod-shaped electrode 6a and having a substantially constant thickness, and dielectric barrier discharge is generated outside the glass tube 6b. I can do it.

  Further, similarly to the electrode unit 2, the sub electrode unit 21 is configured by arranging a plurality of discharge rods 26 in parallel with each other in an annular shape with a predetermined circumferential interval y, and is provided concentrically with the electrode unit 2. It has been. Similarly to the discharge rod 6, the discharge rod 26 is also composed of a rod-shaped electrode 26a such as a stainless steel wire and a cylindrical glass tube 26b surrounding the rod-shaped electrode 26a. A dielectric barrier discharge is performed outside the glass tube 26b. Can be done.

  In addition, the rod-shaped electrode 6a of the discharge rod 6 in the electrode unit 2 is connected to an AC power source 23 via a support structure 24 described later, and the rod-shaped electrode 26a of the discharge rod 26 in the sub-electrode unit 21 is similarly It is grounded through the support structure 24 and the like.

  With the configuration described above, the fastener 38 is removed, the bottom 12b is removed, the electrode unit 2 and the like are incorporated into the container body 12, the bottom 12b is closed again, the lid 13 is opened and closed, and the inside of the discharge container 3 is opened. Then, the mixed gas 37 is supplied to and discharged from the discharge vessel 3 through the sealing plug 18, and the AC is connected between the grounded metal mesh 4, the sub electrode unit 21, and the electrode unit 2. Alternatively, glow discharge occurs when a pulse voltage, in this embodiment an AC voltage is applied.

  In this discharge state, when the discharge vessel 3 surrounded by the anti-floating material 10 is rotated by the rotating device 5 and stirred so that the powder is stirred up by the stirring blades 14, an appropriate plasma is applied to the surface of the flowing powder. Processing can be performed.

  Next, detailed configurations of the electrode unit 2 and the sub electrode unit 21 will be described with reference to FIGS.

  The support structure 24 of the electrode unit 2 and the sub-electrode unit 21 is disposed on the axial center of the cylindrical discharge vessel 3, and the rear end opening 25 b passes through the axial center of the sealing plug 18 described above and the discharge vessel 3. The shaft pipe 25 is inserted into the shaft pipe 25, the front support portion 27 is provided at the front end portion of the shaft pipe 25, and the rear support portion 31 is provided at the rear end portion of the shaft pipe 25.

  Among these, the front end opening 25a of the shaft pipe 25 communicates with the helium gas cylinder 35 and the nitrogen gas cylinder 36, and a cutout groove 18a penetrating in the front-rear direction is formed in the outer peripheral portion of the sealing plug 18. .

  As a result, the mixed gas 37 is injected into the discharge vessel 3 through the shaft pipe 25 from the rear end opening 25b, and then discharged to the outside of the discharge vessel 3 through the notch groove 18a of the sealing plug 18. The inside of the container 3 is always filled with a new mixed gas 37. In addition, the notch groove 18a and the front end opening 25a of the shaft pipe 25 are connected and communicated, and a mixed gas 37 is circulated and used repeatedly by providing a pump in the middle of the ventilation path, thereby reducing gas costs. You may make it plan.

  Further, the front support portion 27 includes a sub attachment support member 28 that attaches and supports the front end portion of the discharge rod 26 of the sub electrode unit 21, and a main attachment support member that attaches and supports the front end portion of the discharge rod 6 of the electrode unit 2. 29, and the sub attachment support member 28 and the main attachment support member 29 are fixed to the inner wall 12a2 of the container body 12 of the discharge vessel 3 by three-point support.

  The sub-mounting support member 28 includes a front base pipe 28a that is externally fitted to the front portion of the shaft pipe 25, a front support member 28b that includes three branch portions 28b1 extending radially from the rear end thereof, And an annular front mounting member 28c formed integrally with the extending end of the branch portion 28b1.

  The main attachment support member 29 includes a front base pipe 29a that is externally fitted to the front base pipe 28a, and a front support member 29b that includes three branch portions 29b1 that come into contact with the front surface of each branch portion 28b1 from the front, An annular front mounting member 29c integrally formed at the extending end of each branch portion 29b1, and the front mounting member 29c is formed to have a larger diameter than the front mounting member 28c of the sub mounting support member 28. Thus, the discharge rod 6 attached to the front attachment member 29c does not interfere with the discharge rod 26 attached to the front attachment member 28c described above.

  The strut member 30 includes a front base pipe 30a that is externally fitted to the front base pipe 29a, and a front support member 30b that includes three branch portions 30b1 that are in contact with the front surface of each branch portion 29b1 from the front. The front support member 30b is formed to have a longer diameter than the front mounting member 29c of the main mounting support member 29, and the container main body of the discharge container 3 via a slip stopper 39 attached to the extending end of the branch portion 30b1. 12 are pressed against the inner wall 12a2 with difficulty in sliding.

  Then, a connecting pin 41 is provided so as to penetrate the shaft pipe 25 in a radial direction from the front base pipes 28a, 29a, 30a that are externally fitted around the shaft pipe 25 in order from the inside, A front support portion 27 having a sub attachment support member 28, a main attachment support member 29, and a projecting member 30 is configured to be able to rotate integrally with the discharge vessel 3.

  In addition, the rear support portion 31 also has a sub-attachment support member 32 that attaches and supports the rear end portion of the discharge rod 26 of the sub-electrode unit 21 and the rear end of the discharge rod 6 of the electrode unit 2, similarly to the front support portion 27. A main attachment support member 33 that attaches and supports the end portion, and a sub attachment support member 32 and a tension member 34 that fixes the main attachment support member 33 to the inner wall 12a2 of the container body 12 of the discharge vessel 3 by three-point support. Have.

  The sub-attachment support member 32 includes a rear base pipe 32a that is externally fitted to the rear portion of the shaft pipe 25, a rear support member 32b that includes three branch portions 32b1 that extend radially from the front end thereof, and each branch. And an annular rear mounting member 32c formed integrally with the extending end of the portion 32b1.

  The main mounting support member 33 includes a rear base pipe 33a that is externally fitted to the rear base pipe 32a, and a rear support member 33b that includes three branch portions 33b1 that are in contact with the rear surface of each branch portion 32b1 from the rear. An annular rear mounting member 33c integrally formed at the extending end of each branch portion 33b1, and the rear mounting member 33c is formed to have a larger diameter than the rear mounting member 32c of the sub mounting support member 32. Thus, the discharge rod 6 attached to the rear attachment member 33c does not interfere with the discharge rod 26 attached to the rear attachment member 32c described above.

  The projecting member 34 includes a rear base pipe 34a that is externally fitted to the rear base pipe 33a, and a rear support member 34b that includes three branch portions 34b1 that are in contact with the rear surface of each branch portion 33b1 from the rear. The rear support member 34b is formed to have a longer diameter than the rear attachment member 33c of the main attachment support member 33, and the container body of the discharge vessel 3 is provided with a slip stopper 39 attached to the extending end of the branch portion 34b1. 12 are pressed against the inner wall 12a2 with difficulty in sliding.

  And like the front support part 27 described above, the shaft pipe 25 is radially fitted from the rear base pipes 32a, 33a, 34a, which are externally fitted around the shaft pipe 25 in order from the inside, A connecting pin 41 is provided so that the rear support portion 31 having the auxiliary mounting support member 32, the main mounting support member 33, and the projecting member 34 can rotate integrally with the discharge vessel 3.

  In addition, when inserting the support structure 24 of the above structure into the container main body 12, the fastener 38 is removed and the bottom part 12b is removed from the main body part 12a.

  Further, in the support structure 24 that can rotate integrally with the discharge vessel 3 in this manner, the front mounting member 29c and the rear mounting member 33c have a plurality of short pipe-like fitting recesses 29c1 and a short pipe-like shape. The plurality of fitting recesses 33c1 are formed to face each other so as to overlap on the same circumference in front view.

  A fitting spring 40 is housed in a compressed state inside the fitting recess 29c1 and the fitting recess 33c1, and the front and rear ends of the discharge rod 6 are inserted into the opposing fitting recess 29c1 and the fitting recess 33c1, respectively. After fitting, the discharge rod 6 can be held by being pressed from the front and back by the mounting spring 40. Thus, the plurality of discharge rods 6 are arranged in an annular shape at a predetermined circumferential interval y in parallel with each other, and the electrode unit 2 is formed.

  Similarly, the front mounting member 28c and the rear mounting member 32c are also provided with a plurality of short pipe-shaped fitting recesses 28c1 and a plurality of short pipe-shaped fitting recesses 32c1 on the same circumference in front view. It is formed to face each other so as to overlap.

  The mounting spring 40 is housed in a compressed state inside the fitting recess 28c1 and the fitting recess 32c1, and the front and rear ends of the discharge rod 26 are inserted into the opposing fitting recess 28c1 and the fitting recess 32c1, respectively. After the fitting, the discharge rod 26 can be held by being pressed from the front and rear by the mounting spring 40. As a result, the plurality of discharge rods 26 are arranged in an annular shape at a predetermined circumferential interval y in parallel with each other, and the sub-electrode unit 21 is formed.

  One end of the discharge rod 6 is pushed into one of the fitting recess 29c1 and the fitting recess 33c1 against the elastic force of the mounting spring 40, and the discharge rod 6 is pulled out from the other while tilting the discharge rod 6. 6 can be removed and the discharge rod 6 can be mounted between the fitting recess 29c1 and the fitting recess 33c1 in the reverse order. The same applies to the discharge rod 26, and the discharge rods 6 and 26 are separate and separable from each other, and can be freely detached from the support structure 24.

  Further, in the front support portion 27, the sub attachment support member 28, the main attachment support member 29, the projecting member 30, and the connecting pin 41 are formed of a conductive material such as stainless steel and insulated from each other. Similarly, the sub attachment support member 32, the main attachment support member 33, the projecting member 34, and the connecting pin 41 are formed of a conductive material such as stainless steel and insulated from each other.

  In the auxiliary mounting support member 28, the front portion of the front base pipe 28a is exposed to the outside through the sealing plug 18 while being externally fitted to the shaft pipe 25. A clip 42 grounded via the wire is locked. Similarly, also in the main attachment support member 29, the front part of the front base pipe 29a is exposed to the outside through the sealing plug 18 while being externally fitted to the front base pipe 28a. A clip 43 connected to the AC power supply 23 via the wire is locked.

  On the other hand, the rod-like electrode 26 a of the discharge rod 26 is connected to the fitting recess 28 c 1 of the front attachment member 28 c in the sub attachment support member 28 via a metal disk 44 between the discharge rod 26. The rod-shaped electrode 6 a of the discharge rod 6 is also connected to the fitting recess 29 c 1 of the front mounting member 29 c in the main mounting support member 29 via the metal disk 44 between the discharge rod 6.

  Thereby, all the discharge rods 6 of the electrode unit 2 are connected to the AC power source 23 via the main attachment support member 29, and all of the discharge rods 26 of the sub electrode unit 21 are connected via the sub attachment support member 28. Can be grounded. At this time, as described above, the wire mesh 4 is also grounded.

  Accordingly, an AC voltage is applied between the wire mesh 4 and the electrode unit 2 to generate glow discharge, and a discharge area 45 is formed in the space between the inner wall 12a2 of the discharge vessel 3 and the glass tube 6b of the discharge rod 6. Is formed.

  Furthermore, an AC voltage is also applied between the electrode unit 2 and the sub-electrode unit 21 to generate glow discharge, and in the space between the glass tube 6b of the discharge rod 6 and the glass tube 26b of the discharge rod 26. However, the discharge region 46 is formed, and the sub-electrode unit 21 functions as a discharge region expansion structure that expands the discharge region of the glow discharge to the inside of the electrode unit 2.

  In the configuration as described above, the rod-shaped electrodes 6a and 26a are covered with the cylindrical glass tubes 6b and 26b having a substantially constant thickness, and a stable glow discharge is generated. This can suppress the breakage of the discharge rods 6 and 26, and the rod-like electrodes 6a and 26a can easily start discharge due to the electric field concentration effect, thereby reducing the burden on the power source.

  Furthermore, thanks to the stable glow discharge, the powder can freely flow between the inside and outside of the electrode unit 2 and the sub-electrode unit 21 through the gap between the discharge rods 6 and 26 that are not likely to be blocked. It is possible to ensure a large powder movement space and to efficiently agitate the powder, and also to allow the powder to flow into the inside of the electrode unit 2 and the sub electrode unit 21.

  In particular, as in this embodiment, when the discharge rods 6 and 26 are separated and can be separated from each other, when the discharge rods 6 and 26 are damaged, the electrode unit 2 and the sub-electrode unit 21 are not damaged. It is only necessary to replace the discharged discharge rods 6 and 26, and when changing the functional group to be added to the powder, the discharge rods 6 and 26 already provided are supplied with predetermined functional groups at the time of discharge. What is necessary is just to replace | exchange for the discharge rod which has a glass tube containing a possible component.

  In addition, during the plasma treatment, all the discharge rods 6 in the electrode unit 2 are equipotential, and all the discharge rods 26 in the sub-electrode unit 21 are all equipotential, so that the discharge rods that are opposed to each other across the center portion. By preventing the glow discharge from occurring between 6 and 26, the inner diameters of the electrode unit 2 and the sub-electrode unit 21 can be increased. In addition, the powder sealed in the discharge vessel 3 freely flows between the inside and outside of the electrode unit 2 and the sub electrode unit 21 through the gap between the discharge rods 6 and 26 while the discharge vessel 3 is rotated. Then, it passes through the stable discharge areas 45 and 46 while being efficiently stirred, and the surface of the powder is uniformly treated.

  Furthermore, by newly forming the discharge area 46 and making the discharge area 45 expandable to the inside of the electrode unit 2, the time for the powder to pass through the discharge area becomes longer, and the plasma irradiation time becomes longer. Thus, the processing time of the plasma processing can be greatly shortened.

  Next, various forms of the cooling structure and the stirring structure in the plasma processing apparatus 1 will be described with reference to FIGS.

First, various forms of the cooling structure will be described.
A sub-electrode unit 21A shown in FIG. 5A has a cooling-type discharge rod 26A disposed in place of a part of the discharge rod 26 of the sub-electrode unit 21 in the plasma processing apparatus 1 described above.

  In the present embodiment, every two discharge rods 26 arranged in an annular shape with a predetermined circumferential interval y in parallel with each other, the discharge rods 26A are arranged. The discharge rod 26A is the same as the normal discharge rod 26 from the viewpoint of reducing the component cost by sharing components, and its end portion is in communication with the shaft pipe 25. A mixed gas 37 as a cooling medium can flow through an internal gap 67 between the electrode 26a and the glass tube 26b.

  Thereby, when the mixed gas 37 is caused to flow through the internal gap 67 of the discharge rod 26A, the discharge rods 26 and 26A of the sub-electrode unit 21A on the center side of the discharge vessel 3 that is difficult to cool can be efficiently cooled.

  A sub-electrode unit 21B shown in FIG. 5B has a cooling pipe 26B dedicated for cooling instead of a part of the discharge rod 26 of the sub-electrode unit 21 in the plasma processing apparatus 1.

  Similarly to the sub-electrode unit 21A, in the plurality of discharge rods 26 arranged in an annular shape at a predetermined circumferential interval y in parallel with each other, the cooling tubes 26B are arranged every two. The cooling tube 26B is formed from a single glass tube 26b in which the rod-shaped electrode 26a is removed from the discharge rod 26 from the viewpoint of component cost reduction by sharing components, and the end portion thereof communicates with the shaft pipe 25. The mixed gas 37 as a cooling medium can flow through the internal space 68 of the glass tube 26b alone.

  Thereby, when the mixed gas 37 is caused to flow into the internal space 68 of the cooling tube 26B, the discharge rod 26 of the sub-electrode unit 21B on the center side of the discharge vessel 3 that is difficult to cool can be efficiently cooled.

  In the plasma processing apparatus 1A shown in FIG. 6A, the sub-electrode unit 21 and the sub-electrode unit 22 are concentric in order from the outside in the space inside the electrode unit 2 in the discharge vessel 3 in which the wire mesh 4 is arranged on the outside. The cooling type discharge cylinder 47 is arranged on the axis 3 a in the discharge vessel 3 inside the innermost sub-electrode unit 22.

  The discharge cylinder 47 is formed of a cylindrical electrode 48 in which a mixed gas 37 or cooling water, which is a cooling medium, can flow in the internal space 52, and a glass cylinder 49 that covers the outer periphery of the cylindrical electrode 48.

  Here, the wire mesh 4, the sub electrode unit 21, and the cylindrical electrode 48 are grounded, and the electrode unit 2 and the sub electrode unit 22 are connected to the AC power source 23. When an AC voltage is applied between the electrode unit 2 and the sub-electrode unit 22, a plurality of discharge areas 45, 46, 50, 51 are continuously formed from the inner wall 12a2 of the discharge vessel 3 to the glass tube 49 to discharge. While the area is greatly expanded, the temperature in the discharge vessel 3 also becomes high.

  Therefore, by supplying the mixed gas 37 or cooling water to the internal space 52 in the cylindrical electrode 48 of the discharge cylinder 47, the discharge rods of the sub-electrode unit 21 and the sub-electrode unit 22 on the center side of the discharge vessel 3 that are difficult to cool. 26 and 53 are efficiently cooled, and the high temperature inside the discharge vessel 3 can be suppressed.

  In the plasma processing apparatus 1B shown in FIG. 6B, a cooling cylinder 55 dedicated to cooling is arranged in place of the discharge cylinder 47 in the plasma processing apparatus 1A described above.

  The cooling cylinder 55 is formed from a single glass cylinder 49 in which the cylindrical electrode 48 is removed from the discharge cylinder 47 described above, and the mixed gas 37 and cooling water as a cooling medium flow through the internal space 54 of the single glass cylinder 49. I can do it.

  Here, the metal mesh 4 and the sub-electrode unit 21 are grounded, and the electrode unit 2 and the sub-electrode unit 22 are connected to the AC power source 23. The metal mesh 4, the sub-electrode unit 21, the electrode unit 2, and the sub-electrode unit 22 Between the inner wall 12a2 of the discharge vessel 3 and the sub-electrode unit 22, a plurality of discharge areas 45, 46, 50 are continuously formed, and the discharge area is similar to the plasma processing apparatus 1A. While greatly expanding, the inside of the discharge vessel 3 also becomes high temperature.

  Therefore, by flowing the mixed gas 37 and cooling water through the internal space 54 of the cooling cylinder 55, the discharge electrodes 26 and 53 of the sub-electrode unit 21 and the sub-electrode unit 22 on the center side of the discharge vessel 3 that are difficult to cool are efficiently used. It is cooled and the high temperature in the discharge vessel 3 can be suppressed.

  When the discharge rods 26, 26A, 53, etc. on the center side of the discharge vessel 3 are efficiently cooled by the sub-electrode units 21A, 21B and the plasma processing apparatuses 1A, 1B shown above, the powder flowing in the discharge vessel 3 Even if the body is a resin or the like, it is possible to reliably prevent welding with each other due to heat accompanying glow discharge, adhesion within the discharge vessel 3, and alteration of the surface.

  A plasma processing apparatus 1 </ b> C shown in FIG. 7 has improved air cooling performance from the outer surface of the discharge vessel 3 in the plasma processing apparatus 1 described above.

  Specifically, the side portions of the left and right support bases 56L and 56R are fixed to the left and right sides of the base 7, respectively, and the discharge vessel 3 is surrounded by the upper surfaces of the support bases 56L and 56R so that the air cooling is performed. An air cooling mechanism 59 is formed by installing the housing 57 and further mounting and fixing an air cooling fan 58 on the upper flat plate portion 57a of the air cooling housing 57.

  In the air-cooled housing 57, left and right intake holes 57b and 57c are opened at the lower portion, and a communication hole 57a1 is opened at the approximate center of the upper flat plate portion 57a in plan view. Further, the air cooling fan 58 has a fan main body 58a made of an electric motor, rotating blades, and the like, and a case 58b surrounding the fan main body 58a. The lower portion of the case 58b communicates with a communication hole 57a1 of the air cooling housing 57. A communication hole 58b1 is opened, and an exhaust hole 58b2 is opened on the side of the case 58b.

  As a result, when the fan main body 58a is driven, air outside the air-cooling housing 57 is sucked from the intake holes 57b and 57c, and then rises along the outer periphery of the discharge vessel 3. From the communication holes 57a1 and 58b1, It passes through 58b and is discharged to the outside through the exhaust hole 58b2. During this time, the discharge vessel 3 and the surrounding metal mesh 4 are directly cooled by air, and the electrode unit 2 and sub-electrode unit 21 inside the discharge vessel 3 are also indirectly cooled.

  Therefore, only by providing such an air cooling mechanism 59, the cooling performance can be enhanced without changing the internal configuration of the discharge vessel 3 as in the sub electrode units 21A and 21B and the plasma processing apparatuses 1A and 1B described above. The cooling structure with excellent versatility can be provided.

Various forms of the stirring configuration will be described.
The stirring blade 60 shown in FIG. 8 is intended to improve the stirring efficiency and extend the plasma irradiation time compared to the stirring blade 14 described above.

  In the stirring blade 60, mounting plates 62, 62 are fixed on the front and rear inner walls of the container body 12 of the discharge vessel 3, and a rake member 63 that is long in the front-rear direction is bridged between the mounting plates 62, 62. The scooping member 63 rotates together with the discharge vessel 3 that rotates in the rotation direction 69.

  The scooping member 63 has a flat plate base 63a on the inner peripheral side in the centrifugal direction and a curved portion 63b on the outer peripheral side in the centrifugal direction, the outer peripheral side in the centrifugal direction is curved toward the rotational direction 69, and the tip of the curved portion 63b. 63c is extended to between the adjacent discharge rods 6.

  Further, a staying plate member 65 is disposed on the outside of the flat plate base portion 63a of the scooping member 63, and a staying discharge portion 64 is formed between the staying plate member 65 and the flat plate base portion 63a described above.

  The stay discharge section 64 has an inflow port 64a provided on the front side in the rotation direction 69 of the scooping member 63 on the inner peripheral side in the centrifugal direction, a stay chamber 64b communicating with the inflow port 64a, and communicating with the stay chamber 64b. At the same time, a discharge port 64c is provided which is located on the outer peripheral side in the centrifugal direction and has a smaller area than the inlet 64a.

  Thereby, the powder 70 scooped up by the scooping member 63 passes through the discharge port 64c from the above-described inflow port 64a via the staying chamber 64b in the middle, and rolls in the centrifugal direction on the curved portion 63b. It spills down from the portion 63 c and gradually flows down into the discharge region 45 through the discharge rod 6.

  Then, when the axial center of the discharge vessel 3 is in a substantially horizontal posture or an inclined posture, the powder 70 accumulated in the lower portion of the discharge vessel 3 is stirred more efficiently than the stirring blade 14 by the rotating stirring blade 60. In addition, after a part is scooped up by the scooping member 63 and flows into the staying chamber 64b from the inlet 64a, the stirring blade 60 rotates together with the discharge vessel 3 and rises from the lower position to the upper position. Since the powder 70 that has flowed in passes through the discharge port 64c and gradually flows through the discharge area 45 due to its own weight, the time for the powder 70 to pass through the discharge area 45 becomes long, and the plasma irradiation time can be lengthened. it can.

  Similarly to the stirring blade 60 described above, the stirring blade 61 shown in FIG. 9 also improves the stirring efficiency and extends the plasma irradiation time.

  In the stirring blade 61, a rake member 66 with a long hole in the front-rear direction is bridged between the aforementioned front and rear mounting plates 62, 62, and the rake member 66 with a hole also rotates in the rotation direction 69. Rotate with container 3

  The rake member 66 with a hole has a flat plate base portion 66a on the inner peripheral side in the centrifugal direction and a flat sieve discharge portion 66b curved in the rotational direction 69 on the outer peripheral side in the centrifugal direction. The tip end portion 66c of the sieve discharge portion 66b extends between the discharge rods 6 and close to the inner wall 12a2 of the vessel main body 12 of the discharge vessel 3 while being curved toward 69. . A large number of discharge holes 66b1 are formed in the rotation direction 69 in the sieve discharge part 66b.

  As a result, the powder 70 scooped up by the holed rake member 66 rolls on the sieve discharge part 66b in the rake member 66, passes through the discharge hole 66b1 described above, and is discharged between the discharge rods 6 through the discharge region 6. It gradually flows down toward 45.

  Then, similarly to the stirring blade 60 described above, when the axial center of the discharge vessel 3 is in a substantially horizontal posture or an inclined posture, the powder 70 in a state of being accumulated at the lower portion of the discharge vessel 3 is efficiently converted by the rotating stirring blade 61. While being stirred well, a part is scooped up by the scooping member 66 with a hole, and while the stirring blade 61 rotates together with the discharge vessel 3 and rises from the lower position to the upper position, it passes through the discharge hole 66b1 and is slightly increased by its own weight. Since the powder 70 flows down and passes through the discharge region 45, the time for the powder 70 to pass through the discharge region 45 becomes longer, and the plasma irradiation time can be made longer.

  Next, another type of plasma processing apparatus 1D will be described with reference to FIGS.

  As shown in FIGS. 10 to 15, the plasma processing apparatus 1 </ b> D differs from the plasma processing apparatus 1 described above in that the discharge region 45 can be expanded outward rather than inward of the electrode unit 2. This is intended to shorten the processing time of the processing.

  In the plasma processing apparatus 1D, similarly to the plasma processing apparatus 1, the discharge rods 6 formed by covering the rod-like electrodes 6a with glass tubes 6b that are cylindrical dielectrics are circularly arranged in parallel with each other at a predetermined circumferential interval y. An electrode unit 2 arranged in an annular shape, and a cylindrical discharge vessel 3A which is arranged outside the electrode unit 2 and encloses powder therein and is formed of glass, and further, this discharge vessel A wire mesh 4 arranged outside 3A and a rotating device 5 for rotating the discharge vessel 3A in a state where glow discharge is generated by applying an AC voltage between the electrode unit 2 and the wire mesh 4 are also provided. .

  Note that the discharge vessel 3A among them has a structure in which the support structure 71 can adjust the radial size by the radial expansion / contraction structures 90 and 91 and the adjustment mechanisms 84 and 85, as described later, and has a small opening. 12Aa, the support structure 71 can be inserted into the container main body 12A. Therefore, unlike the plasma processing apparatus 1, the container main body 12A of the discharge container 3A cannot be divided as an integral part, thereby reducing the number of parts. ing.

  On the other hand, the major difference from the plasma processing apparatus 1 is that the sub-electrode unit 21 is not provided, only the electrode unit 2 is provided, and the support structure 71 of the electrode unit 2 is different from the support structure 24 described above. Is different and the size can be adjusted.

Therefore, the support structure 71 will be described in detail.
The support structure 71 is disposed on the axial center of the cylindrical discharge vessel 3A, and the axial pipe 25 having a rear end opening 25b inserted into the discharge vessel 3A through the axial center of the sealing plug 18, The front support portion 72 is provided at the front end portion of the shaft pipe 25, and the rear support portion 76 is provided at the rear end portion of the shaft pipe 25.

  The front end opening 25 a of the shaft pipe 25 is communicated with the helium gas cylinder 35 and the nitrogen gas cylinder 36, as in the above-described plasma processing apparatus 1, and a notch groove 18 a is formed in the outer peripheral portion of the sealing plug 18. After being injected into the discharge vessel 3A from the shaft pipe 25, the mixed gas 37 is discharged to the outside of the discharge vessel 3A through the notch groove 18a of the sealing plug 18, and the inside of the discharge vessel 3A is discharged. It is always filled with a new mixed gas 37.

  Further, the front support portion 72 supports the discharge rod 6 by attaching the front end portion of the discharge rod 6 to the end surface in the axial direction in the discharge vessel 3A, and can be arranged on the same circumference to form a ring 3. A plurality of arc-shaped mounting members 74, a support member 73 that supports each of the mounting members 74 by one branch 73b, and the support member 73 are supported at three points on the inner wall 12Ab of the container body 12A of the discharge container 3A. And the adjustment mechanism 84 that can change the attachment position of the attachment member 74 with respect to the aforementioned branch part 73b to expand the radial interval.

  In the mounting member 74, a plurality of short pipe-shaped fitting recesses 74 a are formed in an arc shape at predetermined intervals in the rear opening state at the outer peripheral edge portion thereof. On the other hand, a connecting stay 74b is provided on the inner peripheral edge of the mounting member 74 so as to project inward from the middle.

  The support member 73 is externally fitted to the front portion of the shaft pipe 25 described above and is fixed to the shaft pipe 25 by a connecting screw 86, and three support members radially extending from the front end of the base pipe 73a in the radial direction. It has the branch part 73b mentioned above.

  And the tip 73b1 of the branch part 73b is widened, and two long holes 87 are juxtaposed in the circumferential direction, and one long hole 88 is formed in the middle part in the radial direction of the branch part 73b. Has been.

  The projecting member 75 has a rear surface abutted against the front surface of the branch portion 73b, a base block 75a having a thick wall in the axial direction, and a long plate-like projecting member 75b integrally connected to the outside of the base block 75a. The above-mentioned non-slip 39 is also attached to the extended end of the protruding member 75b, and is pressed against the inner wall 12Ab of the container body 12A of the discharge container 3A with difficulty.

  Of these, two screw holes 75a1 are arranged in the radial direction in the base block 75a, and the two adjustment screws 89 are screwed into the screw holes 75a1 through the long holes 88 from the rear. Thus, the projecting member 75 can be fastened to each branch portion 73 b of the support member 73.

  Thus, after loosening the two adjusting screws 89, the adjusting screw 89 is slid to the inner periphery of the long hole 88, and the projecting member 75 is expanded and contracted in the radial direction with respect to the branch portion 73b. When the outer end 75b1 of the member 75 reaches a predetermined radial position, the two adjusting screws 89 are tightened, and the projecting member 75 is fastened to the branch portion 73b so that the projecting member 75 can be freely set to a predetermined length. Can be expanded and contracted to form a radially expandable structure 90.

  The adjustment mechanism 84 includes a radial expansion / contraction structure 80 that expands / contracts the attachment member 74 in the radial direction with respect to the branch portion 73b, and a circumferential movement structure 81 that changes a circumferential interval between the adjacent attachment members 74.

  Of these, in the radially extending and contracting structure 80, two screw holes 74b1 are juxtaposed in the circumferential direction on the inner peripheral edge of the connecting stay 74b of the mounting member 74, and the two adjusting screws 92 are connected from the rear. The attachment member 74 can be fastened to each branch portion 73b of the support member 73 by being screwed into the screw hole 74b1 through the long hole 87 described above.

  As a result, after loosening the two adjusting screws 92, the adjusting screw 92 is slid along the inner periphery of the elongated hole 87, and the mounting member 74 is expanded and contracted in the radial direction with respect to the branch portion 73 b, thereby mounting the mounting member 74. When the fitting recess 74a provided at the position reaches a predetermined radial position, the two adjustment screws 92 are tightened, and the mounting member 74 is fastened to the branch portion 73b so that the mounting member 74 can be freely set to a predetermined length. Can be expanded and contracted.

  In the circumferential movement structure 81, a coupling hole 74 c is drilled at the circumferential end of the inner peripheral edge of the mounting member 74, while a coupling plate 94 is disposed on the back of the circumferential end of the mounting member 74. A cutout 94a is formed at one end of the connecting plate 94, and a through hole 94b is drilled at the other end. Two adjusting screws 93 are connected from the rear through the cutout 94a and the through hole 94b. By screwing into the holes 74c, the circumferential ends of the adjacent mounting members 74 can be fastened.

  Thereby, after loosening the adjustment screw 93 which is passed through the notch 94a out of the two adjustment screws 93, the adjustment screw 93 is slid to the inner periphery of the notch 94a, so that the mounting member 74 is attached. Is moved in the circumferential direction, and then the adjustment screw 93 that is passed through the notch 94a is tightened so that the adjacent mounting members 74 are fastened via the connecting plate 94, so that the circumference of the adjacent mounting members 74 is The direction interval can be changed freely.

  Similarly to the front support portion 72 described above, the rear support portion 76 also supports the discharge rod 6 and is arranged on the same circumference with three arcuate mounting members 78 that can form a ring. The support member 77 that supports the attachment member 78 by the branch portion 77b, the strut member 79 that fixes the support member 77 to the inner wall 12Ab of the discharge vessel 3A, and the attachment position of the attachment member 78 to the branch portion 77b described above. And an adjustment mechanism 85 capable of expanding the radial interval by changing.

  Also in the mounting member 78, a plurality of short pipe-shaped fitting recesses 78 a are formed in an arc shape at a predetermined interval in the front opening state, while the inner peripheral edge portion of the mounting member 78 has a middle portion thereof. A connecting stay 78b protrudes inward.

  The support member 77 also has a base pipe 77a that is fixed to the shaft pipe 25 by a connecting screw 86, and three branch portions 77b that extend radially from the rear end of the base pipe 77a. The tip 77b1 of the branch 77b has two long holes 95 arranged in the circumferential direction, and one long hole 96 is formed in the middle of the branch 77b in the radial direction.

  The strut member 79 also has a front surface abutted against the rear surface of the branch portion 77b, a thick base block 79a in the axial direction, and a long plate-like protruding member 79b integrally connected to the outside of the base block 79a. The anti-slip 39 is also attached to the extending end of the protruding member 79b, and is pressed against the inner wall 12Ab of the container body 12A of the discharge vessel 3A with difficulty.

  Of these, the base block 79a also has two screw holes 79a1 arranged in the radial direction, and the two adjustment screws 89 are screwed into the screw holes 79a1 through the long holes 96 from the front, The tension member 79 can be fastened to each branch portion 77 b of the support member 77.

  Thus, after loosening the two adjusting screws 89, the adjusting screw 89 is slid to the inner periphery of the long hole 96, and the protruding member 79 is expanded and contracted in the radial direction with respect to the branch portion 77b. When the outer end 79b1 of the member 79 reaches a predetermined radial position, the two adjusting screws 89 are tightened, and the projecting member 79 is fastened to the branch portion 77b so that the projecting member 79 can be freely set to a predetermined length. The elastic member 91 in the radial direction of the strut member 75 is formed.

  By providing the radial expansion / contraction structure 91 of the rear support portion 76 and the radial expansion / contraction structure 90 of the front support portion 72 described above, plasma treatment is performed using various discharge vessels 3A having different inner diameters of the container main body 12A. The apparatus 1D can be manufactured, it becomes possible to cope with various apparatus specifications, and versatility is improved.

  The adjustment mechanism 85 also includes a radial expansion / contraction structure 82 that expands / contracts the attachment member 78 in the radial direction, and a circumferential movement structure 83 that changes a circumferential interval between the adjacent attachment members 78.

  Among these, in the radially extending and contracting structure 82, two screw holes 78b1 are arranged in the circumferential direction on the inner peripheral edge of the connecting stay 78b of the mounting member 78, and the two adjusting screws 92 are connected from the front. The attachment member 78 can be fastened to each branch portion 77 b of the support member 77 by screwing into the screw hole 78 b 1 through the long hole 95.

  Thereby, after loosening the two adjusting screws 92, the adjusting member 92 is slid to the inner periphery of the elongated hole 95, and the attaching member 78 is expanded and contracted in the radial direction with respect to the branch portion 77b, thereby attaching the attaching member 78. When the fitting recess 78a provided at the position reaches a predetermined radial position, the two adjusting screws 92 are tightened, and the mounting member 78 is fastened to the branch portion 77b so that the mounting member 78 can be freely set to a predetermined length. Can be expanded and contracted.

  In the circumferential movement structure 83, a coupling hole 78 c is drilled at the circumferential end of the inner peripheral edge of the mounting member 78, while a coupling plate 97 is disposed on the front surface of the circumferential end of the mounting member 78. A cutout 97a is formed at one end of the connecting plate 97, and a through hole 97b is drilled at the other end. Two adjusting screws 93 are connected from the front through the cutout 97a and the through hole 97b. By screwing into the holes 78c, the circumferential ends of the adjacent mounting members 78 can be fastened.

  Accordingly, after loosening the adjustment screw 93 that is passed through the notch 97a out of the two adjustment screws 93, the adjustment screw 93 is slid to the inner periphery of the notch 97a, so that the mounting member 78 is attached. Is moved in the circumferential direction, and then the adjustment screw 93 that is passed through the notch 97a is tightened so that the adjacent mounting members 78 are fastened via the connecting plate 94, so that the circumference of the adjacent mounting members 78 is The direction interval can be changed freely.

  In the above-described configuration, both the front support portion 72 and the rear support portion 76 are fixed to the common shaft pipe 25 by the connecting screw 86 via the base pipes 73a and 77a, and the tension members 75 and 79 are fixed. Is fixed to the inner wall 12Ab of the discharge vessel 3A, and the support structure 71 can rotate integrally with the discharge vessel 3A.

  Further, the fitting recess 74a of the mounting member 74 and the fitting recess 78a of the mounting member 78 are formed to face each other so as to overlap on the same circumference when viewed from the front, and the fitting recess 74a, The discharge rod 6 is pressed and held from the front and rear by a mounting spring 40 housed in a compressed state inside 78a so that it can be detached from the support structure 71 as necessary.

  As shown in FIGS. 10, 15, and 16, in the plasma processing apparatus 1 </ b> D having such a support structure 71, as in the plasma processing apparatus 1, all of the discharge rods 6 of the electrode unit 2 are mounting members. 74, the support member 73, the shaft pipe 25, and the clip 98 are connected to the AC power supply 23, while the wire mesh 4 is grounded, and an AC voltage is applied between the wire mesh 4 and the electrode unit 2. As a result, glow discharge occurs and a discharge region 45 is formed.

  Therefore, in the above-described circumferential movement structures 81 and 83, in the above-described radial expansion and contraction structures 80 and 82 in a state where the adjustment screw 93 is loosened and the adjacent mounting members 74 and 78 can move in the circumferential direction. The adjustment screw 92 is loosened, and the attachment members 74 and 78 are expanded and contracted in the radial direction.

  For example, as shown in FIG. 16, the position of the shaft pipe 25, the support member 77, the discharge vessel 3 </ b> A, etc. is kept as it is, and after the adjustment screw 93 is loosened, the adjustment screw 92 is loosened and the inside of the elongated hole 95 of the support member 77. When the circumferential surface is slid inward in the order of position 99, position 100, and position 101, the end surface of the support member 77 moves outward in the circumferential direction in the order of position 102, position 103, and position 104, and adjacent supports. While the circumferential interval of the member 77 becomes narrow, the outermost surface of the glass tube 6b moves inward in the order of the position 105, the position 106, and the position 107.

  As a result, the radial interval x between the discharge vessel 3A as the first dielectric and the glass tube 6b of the discharge rod 6 as the second dielectric increases to x1, x2, and x3. The discharge area 45 of the glow discharge is expanded outward from the electrode unit 2. In other words, the front and rear support portions 72 and 76 function as a discharge area expansion structure, the time for the powder to pass through the discharge area 45 is lengthened, the plasma irradiation time is lengthened, and the plasma treatment time is greatly shortened. be able to.

  Next, another type of plasma processing apparatus 1E will be described with reference to FIGS.

  As shown in FIGS. 17 and 18, this plasma processing apparatus 1E differs from the above-described plasma processing apparatus 1D in that it facilitates replacement of the discharge rod 6, particularly the glass tube 6b, thereby maintaining the electrode unit 2 in maintainability. In addition, it is intended to further improve the immediate response to functional group changes.

  Similarly to the plasma processing apparatus 1D, this plasma processing apparatus 1E is also disposed with an electrode unit 2 in which discharge rods 6 are arranged in parallel to each other in an annular shape, and disposed outside the electrode unit 2, and powder is enclosed inside. A cylindrical discharge vessel 108 made of glass, and a stainless steel metal film 109 disposed outside the discharge vessel 108, and between the electrode unit 2 and the metal film 109. The rotating device 5 is also provided for rotating the discharge vessel 108 in a state in which glow discharge is generated by applying an AC voltage to the discharge vessel 108.

  On the other hand, the major difference from the plasma processing apparatus 1D is that the structure of the support structure 110 of the electrode unit 2 is different from that of the support structure 71 described above.

Therefore, the support structure 110 will be described in detail.
The support structure 110 includes a main body portion 110a having a current path and a ventilation path, and a support member 110b for inserting and fixing the rear end portion of the discharge rod 6 while fixing the front end portion of the discharge rod 6. The

  In the main body 110 a, a gas pipe 111 communicating with the helium gas cylinder 35 and the nitrogen gas cylinder 36 is provided, and the rear end of the gas pipe 111 is made of stainless steel disposed on the axial center of the discharge vessel 108. The pipe 113 is connected to the front end through a universal joint 112.

  The rear end of the pipe 113 is connected in communication with a central portion of a stainless steel disk 114 disposed on the axis of the discharge vessel 108, and the disk 114 is a short circle disposed on the axis of the discharge vessel 108. It is fastened and fixed to a front surface of the columnar support block 115 by a plurality of fixing screws 118 through a seal member 123 such as packing. On the other hand, a carbon bearing 126 is fitted around the middle of the pipe 113, and this bearing 126 is connected to the AC power supply 23 via a lead wire 116 and the like.

  A concave portion 115a that opens forward is formed in the front central portion of the front portion of the support block 115, and the front end of an insertion hole 115b that penetrates the support block 115 in the front-rear direction is formed in the front peripheral portion of the concave portion 115a. Is communicated.

  A flange portion 115d protrudes in the radial direction from the front peripheral portion of the front half of the support block 115, while the front peripheral portion of the rear half of the support block 115 has a front and rear intermediate portion on the outer peripheral side surface. A groove 115c communicating with the rear end is formed, and a filter 122 is attached to the rear end of the groove 115c.

  Here, the discharge vessel 108 has a cylindrical shape with the rear end closed by the lid 119 and the front opened, and a flange portion 108a projects in the radial direction at the front end.

  As a result, the discharge vessel 108 is moved from the rear toward the support block 115 and is slid while being externally fitted to the rear half of the support block 115, and the flange portion 108a of the discharge vessel 108 is moved to the flange portion 115d of the support block 115. After the contact, the connecting band 121 is wound so as to straddle between both flange portions 115 d and 108 a, and the discharge vessel 108 can be detachably attached to the support block 115 by the set screw 120.

  Furthermore, the discharge rod 6 is inserted into the aforementioned insertion hole 115b from the rear in an airtight manner through a seal member 127 such as packing, but the rod-like electrode 6a of the discharge rod 6 penetrates the disk 114. The protruding end is fixed to the front surface 114a of the disk 114 by welding or the like. On the other hand, the tip of the glass tube 6b of the discharge rod 6 is brought into contact with a ring 128 that is fitted on the front of the rod-like electrode 6a so as to be slidable back and forth, and this ring 128 is inserted into the insertion hole from the recess 115a. The mounting spring 125 wound around the rod-like electrode 6a up to the front part 115b is urged rearward.

  The support member 110b has a ring shape, and the outer peripheral side surface thereof is fixed to the rear portion of the inner wall 108b of the discharge vessel 108. An insertion hole 129 and a vent hole 130 having a smaller diameter than that of the insertion hole 129 are coaxially arranged in the front-rear direction of the support member 110b. The filter 124 is attached.

  Accordingly, when the discharge vessel 108 is mounted on the support block 115, the rear end portion of the glass tube 6b of the discharge rod 6 is inserted into the support member 110b from the front, and then attached by the mounting spring 125 stored in a compressed state. The front end of the glass tube 6b is pressed rearward through the ring 128 and slid back and forth along the rod-shaped electrode 6a fixed to the disk 114, so that the discharge rod 6 is connected to the main body 110a and the support member 110b. Can be held in between.

  In the configuration as described above, when the discharge vessel 108 is mounted on the support block 115, the discharge rods 6 are arranged in an annular shape at a predetermined circumferential interval in parallel with each other to form the electrode unit 2.

  After that, when the mixed gas 37 is supplied to the gas pipe 111, the mixed gas 37 is injected into the insertion hole 115 b through the universal joint 112, the pipe 113, and the recess 115 a of the support block 115, and the rod-shaped electrode in the discharge rod 6. After passing through the vent hole 130 from the internal gap 131 between the glass tube 6 b and the glass tube 6 b, it is filtered by the filter 124 and then injected into the discharge vessel 108. At this time, the electrode unit 2 is efficiently air-cooled by the mixed gas 37. Thereafter, the mixed gas 37 used for the plasma treatment flows into the groove 115c through the filter 122 provided in the support block 115, and is discharged out of the discharge vessel 108 from the outer periphery of the flange 115d.

  When an alternating voltage is applied between the metal film 109 and the electrode unit 2 while filling the mixed gas 37 in the discharge vessel 108 in this way, glow discharge occurs, and the inner wall 108b of the discharge vessel 108 and the discharge rod A discharge area 45 is formed in the space between the six glass tubes 6b. Then, in the discharge vessel 108 rotated by the rotating device 5, the powder freely flows between the inside and outside of the electrode unit 2, and passes through the stable discharge region 45 while being efficiently stirred, so that the surface of the powder is all over. Uniformly processed.

  As shown in FIGS. 17 and 19, in such a plasma processing apparatus 1D, when the discharge rod 6 is replaced, first, after loosening the set screw 120 and removing the connecting band 121 (arrow 132), the inside and outside Then, the discharge vessel 108 with the support member 110b and the metal film 109 fixed thereto is pulled out rearward from the support block 115 (arrow 133).

  Then, the rear end portion of the glass tube 6b of the discharge rod 6 is removed from the insertion hole 129 of the support member 110b, and the discharge rod 6 is left on the support block 115 side and is exposed. For this reason, access to the damaged discharge rod 6 is simplified, and repair and replacement thereof are facilitated.

  In particular, when the functional group to be added to the powder is changed, only the glass tube 6b is inserted into the insertion hole of the support block 115 while the rod-like electrode 6a having the tip fixed to the disk 114 is left on the support block 115 side. The glass tube 6b can be easily replaced with one suitable for generating a predetermined functional group by pulling backward from 115b.

  Next, another type of plasma processing apparatus 1F will be described with reference to FIGS.

  Unlike the above-described plasma processing apparatus 1E, this plasma processing apparatus 1F uses an agitating blade 144 to connect an electrode structure 142 incorporating the electrode unit 2A, its support structure, current path, ventilation path, and the like into a discharge vessel 140. By making it easy to attach and detach, the component cost is reduced, the maintainability is improved, and the assembling time and processing time are shortened.

  As shown in FIG. 20, similarly to the plasma processing apparatus 1E, this plasma processing apparatus 1F is also provided with an electrode unit 2A in which discharge rods 6A are arranged in an annular shape parallel to each other, and on the outside of the electrode unit 2A. The body 70 is sealed inside, and includes a cylindrical discharge vessel 140 formed of glass, and further, a stainless steel metal film 109 disposed outside the discharge vessel 140 and the electrode unit 2A. The rotating device 5 is also provided for rotating the discharge vessel 140 in a state where glow discharge is generated by applying an AC voltage between the metal film 109 and the metal film 109.

  On the other hand, the major difference from the plasma processing apparatus 1E is that the structure of the electrode structure 142 is different from that of the support structure 110 described above.

Therefore, the electrode structure 142 will be described in detail.
As shown in FIGS. 20 and 21, the electrode structure 142 closes the electrode unit 2A and the opening 140a at the front end of the bottomed cylindrical discharge vessel 140 whose rear end is closed and the electrode unit 2A. The agitation blade 144 interposed between the discharge unit 6A adjacent to the electrode unit 2A and the lid unit 143 that supports the structure are integrally incorporated.

  Among these, the lid unit 143 closes the opening 140a, supports and fixes the front end portions of the electrode unit 2A and the stirring blade 144, and includes the main body portion 143a having a current path and a ventilation path, and the electrode unit 2A and the stirring blade 144. And a support member 143b for supporting and fixing the rear end portion.

  As shown in FIGS. 20 to 22 and 24, the main body 143a includes a lid 145 having a disk 179, which is a resin lid disposed on the axis 147 of the discharge vessel 140, and the lid 145. It has a plug part 146 that can be opened and closed in a hole 179a formed on the axis 147 of the disk 179.

  In the lid portion 145, the outer peripheral portion of the back surface 179c of the disk 179 is airtightly connected to the front surface of the flange portion 140a1 protruding in the radial direction from the front end of the discharge vessel 140 via a seal member 148 such as packing. It is detachably clamped and fixed by a fixing tool 149 so that the opening 140a of the discharge vessel 140 can be closed by a disk 179.

  And on the back surface 179c of the disk 179, three arcuate conductive mounting members 150 arranged on the same circumference and capable of forming a ring are provided on the radially inner side of the circumferential end portion. The plurality of conductive bolts 151 are fastened and fixed. Then, the front end portion of the discharge rod 6A is attached and supported on the outer side in the radial direction of the mounting member 150, and the stirring blade 144 is disposed between the circumferential end portions of the adjacent mounting members 150, as described above. In addition, it can be interposed between adjacent discharge rods 6A.

  Further, a flange portion 152a at the rear end of the support cylinder 152 disposed on the shaft center 147 is formed on the outer surface of the hole 179a on the surface 179b of the disk 179, and a plurality of conductive bolts via a seal member 153 such as packing. The support cylinder 152 is integrated with the disk 179 so as to be fastened and fixed in an airtight manner by the 154 and normally communicated with the hole 179a. The conductive bolt 154 is connected to the above-described conductive bolt 151 in which the attachment member 150 is fastened and fixed to the disk 179 via the lead wire 155.

  In the plug portion 146, a cylindrical conductive introduction pipe portion 157 having a ventilation path 157a formed on the shaft center 147 and a cylindrical conductive exhaust having a ventilation path 158a formed on the same shaft center 147. A pipe portion 158 is connected to the front and rear.

  Then, a conductive connector 171 is interposed between the flange portion 157e at the rear end of the introduction pipe portion 157 and the flange portion 158b at the front end of the exhaust pipe portion 158 so that the flange portions 157e and 158b are separated from each other. In this state, the intake and exhaust pipe 159 in which the introduction pipe portion 157 and the exhaust pipe portion 158 are integrated is formed by fastening with the bolt 165. Further, a vent path 170 extending in the radial direction is formed between the flange portions 157e and 158b, and the inner end of the vent path 170 is communicated with the front end of the vent path 158a of the exhaust pipe portion 158 described above.

  In the introduction pipe portion 157, a gas pipe 161 communicated with the helium gas cylinder 35 and the nitrogen gas cylinder 36 is communicated with the front end opening 157b via a universal joint 162.

  A ring-shaped outer peripheral groove 157c is formed in front of the flange portion 157e in the introduction pipe portion 157, and a carbon bearing 160 is externally fitted in the outer peripheral groove 157c. It is connected to the AC power source 23 via a line 163. The bearing 160 is slidably attached to the outer circumferential groove 157c by sandwiching the outer circumferential groove 157c between the left and right carbon blacks 160a and 160b and fastening the carbon black 160a and 160b with upper and lower bolts 168. It is fitted.

  On the other hand, the front end 164a of the introduction pipe 164 extending in the front-rear direction is connected to the rear end opening 157d of the introduction pipe portion 157 so as to be able to communicate. The rear end opening 164b of the introduction pipe 164 passes through the hole 179a of the disk 179. It is inserted into the discharge vessel 140.

  The exhaust pipe portion 158 is concentrically disposed inside the support cylinder 152 of the lid portion 145 described above, and a male screw is threaded on the outer peripheral surface of the exhaust pipe portion 158, so that the inner peripheral surface of the support cylinder 152 Is internally threaded, and the exhaust pipe 158 can be removably screwed into the support cylinder 152. Further, a seal member 156 such as an O-ring is fitted and fixed to the corner of the flange portion 158b of the exhaust pipe portion 158. When the exhaust pipe portion 158 is rotated and screwed into the support cylinder 152, it is fastened. The seal member 156 is brought into contact with the inner side of the front end of the support cylinder 152 so that the exhaust pipe 158 and the support cylinder 152 are screwed in an airtight manner.

  A front end 166a of an exhaust pipe 166 disposed concentrically outside the introduction pipe 164 is connected to the rear end opening 158c of the exhaust pipe portion 158 so as to communicate with the rear end opening 158c. The space between the end 166b and the outer peripheral side surface of the middle portion of the introduction pipe 164 is airtightly closed.

  Further, a large number of exhaust holes 166c penetrating in the radial direction are formed on the outer peripheral side surface of the exhaust pipe 166, and the bag-shaped filter 167 is covered so as to cover all of the exhaust holes 166c from the outside. It is installed.

  In the configuration as described above, the opening 140a of the discharge vessel 140 is closed by the disk 179 of the lid portion 145, the exhaust pipe portion 158 is screwed into the support cylinder 152, and the plug portion 146 is attached to the lid portion 145. After that, when the helium gas cylinder 35 and the nitrogen gas cylinder 36 are opened, the mixed gas 37 is introduced into the plug part 146 by the gas pipe 161, the universal joint 162, the introduction pipe part 157, the introduction path 157 a, and the introduction pipe 164. 173 is injected into the discharge vessel 140 through the rear end opening 164b of the introduction pipe 164. Thereafter, the injected mixed gas 37 is discharged from the intake / exhaust pipe 159 through the filter 167, the exhaust hole 166c, the exhaust pipe 166, the ventilation path 158a of the exhaust pipe section 158, and the exhaust ventilation path 174 including the ventilation path 170. It is discharged out of the container 140. In this way, the inside of the discharge vessel 140 can always be filled with the new mixed gas 37.

  Further, the lead wire 163 connected to the AC power source 23 is connected to the disk 179 via the carbon bearing 160 in the plug portion 146, the introduction pipe portion 157, the coupling tool 171, the exhaust pipe portion 158, and the support cylinder 152. The conductive bolt 154 is connected to a mounting member 150 via a lead wire 155 and a conductive bolt 151, and the front end is connected to the mounting member 150 as will be described later. An AC voltage can be applied between the electrode unit 2 </ b> A including the discharge rod 6 </ b> A to which the portion is attached and the metal film 109 described above.

  As a result, the plug portion 146 can be formed so that it can be opened and closed in the hole 179a of the disk 179, and the current path for glow discharge and the ventilation paths 173 and 174 are integrally incorporated. Current paths and ventilation paths 173 and 174 are concentrated on the plug portion 146 constituting the electrode structure 142, and simultaneously with the insertion of the electrode structure 142, the current paths and ventilation paths 173 and 174 are connected to the plasma processing apparatus 1F. Can be easily and quickly assembled, the time required for assembling the plasma processing apparatus 1F can be shortened, and the working efficiency can be improved.

  As shown in FIGS. 20, 22, and 23, the support member 143 b described above is disposed on the rear shaft center 147 in the discharge vessel 140 and is made of resin and formed in a ring shape.

  The discharge rod 6A is sandwiched between the front surface on the radially outer side of the support member 143b and the rear surface on the radially outer side of the mounting member 150 as described in detail later.

  Further, on the circumferential direction of the front surface of the support member 143b, the rear end portions 144b of the three stirring blades 144 are in contact with each other at a predetermined circumferential interval from the front, and each of the two bolts 169 is screwed from the rear. Thus, it is fastened and fixed to the support member 143b. On the other hand, the front end portion 144a of the stirring blade 144 is brought into contact with the rear surface 179c of the disk 179 from the rear at the same circumferential interval, and is fastened and fixed to the disk 179 by two bolts 172 that are screwed from the front. ing.

  As a result, the support member 143b of the lid unit 143 is firmly connected to the disk 179 of the main body 143a of the lid unit 143 via the three stirring blades 144, and then the attachment member 150 provided on the disk 179 The electrode structure 142 in which the electrode unit 2A, the lid unit 143, and the stirring blade 144 are integrally incorporated can be configured so as to sandwich the discharge rod 6A between the support member 143b.

  Further, as shown in FIGS. 20, 22, 23, and 25 (a), the electrode unit 2A is configured by arranging a plurality of discharge rods 6A in parallel with each other in an annular shape at a predetermined circumferential interval. Has been.

  The discharge rod 6A includes a rod-shaped electrode 6a such as a stainless wire, a glass tube 6b that surrounds the rod-shaped electrode 6a and has a substantially constant thickness, and is fitted and fixed to the front and rear ends of the rod-shaped electrode 6a. Consists of ring-shaped front and rear locking members 175 and 176 such as conductive push nuts that hold the glass tube 6b in a predetermined position on the rod-shaped electrode 6a by abutting the side surfaces with both end surfaces of the glass tube 6b. Is done.

  Further, the mounting member 150 and the support member 143b that sandwich the discharge rod 6A from the front and the back are respectively provided with a plurality of short pipe-shaped fitting recesses 150a and a plurality of short pipe-shaped fitting recesses 143b1 in front view. The outermost peripheral portions are formed to face each other so as to overlap on the same circumference.

  On the same axis of the fitting recess 150a, a small-diameter hole 150a1 smaller in diameter than the locking member 175 abutted on the front end surface of the crow pipe 6b and a large-diameter hole larger in diameter than the locking member 175 are provided. 150a2 is connected to the front and rear.

  On the other hand, the fitting recess 143b1 is formed to have a larger diameter than the locking member 176 that contacts the rear end surface of the glass tube 6b. Further, an attachment spring 177 is interposed in a compressed state between the locking member 176 and the bottom surface of the fitting recess 143b1.

  Thus, when the electrode structure 142 is assembled, the discharge rod 6A is pressed forward via the locking member 176 by the mounting spring 177 housed in the fitting recess 143b1 in a compressed state, and the fitting recess 150a is large. The discharge rod 6A can be stably held between the mounting member 150 and the support member 143b by sliding the inner wall of the diameter hole 150a2 and the fitting recess 143b1.

  Further, even after the electrode structure 142 is assembled, the discharge rod 6A is pushed backward against the elastic force of the mounting spring 177, so that the front end of the discharge rod 6A has a large diameter of the fitting recess 150a. The discharge rod 6A can be removed from the attachment member 150 and the support member 143b and replaced by being detached from the hole 150a2.

  In addition, the rod-shaped electrode 6a of the discharge rod 6A is connected to the mounting member 150 via the locking member 175. Therefore, as described above, an AC voltage is applied between the electrode unit 2A and the metal film 109. can do.

  Further, as shown in FIGS. 20 to 23, the stirring blade 144 is formed in the shape of a long plate as described above, but the radially outer axial side edge portion 144c that contacts the inner wall 140b of the discharge vessel 140 is formed. Is formed in a U-shape opened inward in front sectional view.

  Thus, when the assembled electrode structure 142 is inserted into the discharge vessel 140, the axial side edge portion 144c of the three stirring blades 144 slides smoothly while contacting the inner wall 140b of the discharge vessel 140. Then, the electrode structure 142 is guided to a predetermined position. That is, the electrode structure 142 is held at a predetermined position with respect to the discharge vessel 140 only through the stirring blade 144 and is configured as a separate body that can be separated from the discharge vessel 140.

  For this reason, the electrode structure 142 is inserted into the discharge vessel 140 while the three stirring blades 144 are slid on the inner wall 140b of the discharge vessel 140, and is incorporated into the electrode structure 142 together with the stirring blade 144. The discharge rod 6A of the electrode unit 2A is also held at a predetermined radial position from the inner wall 140b, and the electrode unit 2A can be supported at an appropriate position using the stirring blade 144. A complicated support structure such as the structure 110 is not necessary, so that the cost of parts can be reduced and the maintainability can be improved.

  Further, the lid unit 143 incorporated in the electrode structure 142 together with the stirring blade 144 is also held at a predetermined position with respect to the discharge vessel 140, and the lid unit for the discharge vessel 140 using the stirring blade 144. The positioning of 143 can be performed quickly, and the assembly time required for assembling the plasma processing apparatus 1F is shortened.

  Also, as shown in FIGS. 20 to 22 and FIG. 25 (b), the conductive bolt 151 is inserted through the disk 179 into the long hole 150b of the mounting member 150, and the nut 181 is screwed to the tip thereof. Thus, the attachment member 150 is fastened and fixed to the disk 179.

  And since this long hole 150b is formed long in the radial direction, the conductive bolt 151 is loosened to move each mounting member 150 in the radial direction, and when the predetermined radial position is reached, the conductive bolt 151 is tightened again. Thus, the radial position of the large-diameter hole 150a2 to which the front end portion of the discharge rod 6A is attached can be adjusted.

  On the other hand, the support member 143b in which the fitting recess 143b1 is formed is detached from the stirring blade 144 of the electrode structure 142 by loosening the bolt 169 described above, so that the fitting recess 143b1 is at a predetermined radial position. After the replacement, by tightening the bolt 169 again, the radial position of the fitting recess 143b1 to which the rear end portion of the discharge rod 6A is attached can be adjusted.

  Thus, by adjusting the radial position of the large diameter hole 150a2 and the fitting recess 143b1, the diameter between the discharge vessel 140 as the first dielectric and the glass tube 6b of the discharge rod 6A as the second dielectric. In this case, the long hole 150b of the mounting member 150 and the detachable support member 143b function as a discharge area expansion structure, and the time for the powder 70 to pass through the discharge area becomes longer, and the plasma is increased. By extending the irradiation time, the plasma processing time can be significantly reduced.

  Further, the supply configuration and the extraction configuration of the powder 70 when the electrode structure 142 configured as described above is used will be described with reference to FIGS. 20 and 26 to 28.

Among these, the supply structure of the powder 70 is demonstrated.
As shown in FIGS. 20 and 26, before placing the discharge container 140 on the rotating device 5, the discharge container 140 with the metal film 109 wound outside is erected with its opening 140a facing upward. Let

  On the other hand, the front end portion 144a of the three stirring blades 144 is fastened and fixed to the back surface 179c of the disk 179 in the main body portion 143a of the lid unit 143 by a bolt 172, and further, a ring-like shape is attached to the rear end portion 144b of the stirring blade 144 The support member 143b is fastened and fixed with a bolt 169. Thereafter, the upper end of the discharge rod 6A was fastened and fixed to the back surface 179c of the disk 179 while the lower end of the discharge rod 6A was pushed down in the fitting recess 143b1 of the support member 143b against the elastic force of the mounting spring 177. By inserting the discharge rod 6A between the attachment member 150 and the support member 143b so as to be inserted into the large-diameter hole 150a2 of the attachment member 150, the base structure portion 178 excluding the plug portion 146 from the electrode structure 142. Form.

  Subsequently, while sliding the axial side edge portion 144c of the stirring blade 144 on the inner wall 140b of the discharge vessel 140, the foundation structure portion 178 is inserted into the discharge vessel 140 from the opening 140a, and the outer periphery of the disk 179 is discharged. After the foundation structure 178 is lowered until it comes into contact with the flange 140a1 of the container 140, the disk 179 is clamped and fixed to the discharge container 140 by the above-described fixture 149, and the foundation structure 178 is discharged first. It is inserted into the container 140.

  Thereafter, as shown in FIG. 27, the outlet 180a of the funnel 180 is inserted into the support cylinder 152 standing from the hole 179a of the disk 179, and the powder 70 is passed from the hole 179a into the discharge vessel 140 through the funnel 180. Pour and supply. Subsequently, the plug 146 is held by holding the connector 171 and inserted into the discharge vessel 140 from the support cylinder 152 with the introduction pipe 164 facing down, while the exhaust pipe of the plug 146 is inserted into the support cylinder 152. The plug portion 146 is attached to the lid portion 145 by screwing the portion 158.

  Thus, when supplying the powder 70 before the plasma treatment, if the electrode structure 142 is to be inserted in a state where the powder 70 is stored in the discharge vessel 140, the electrode structure 142 is attached to the tip of the electrode structure 142. When the tip of the electrode structure 142 interferes with the powder 70 on the bottom surface 140c and the electrode structure 142 cannot be inserted because the distance between the support member 143b and the bottom surface 140c of the discharge vessel 140 is small. Even if it exists, the powder 70 can be easily supplied into the discharge vessel 140 without causing interference with the electrode structure 142.

  Further, even when the powder 70 is replenished during the plasma processing, the exhaust pipe portion 158 is rotated in the direction opposite to the fastening direction in the assembled electrode structure 142 in the reverse order to that shown in FIG. By removing from 152 and opening the hole 179a of the disk 179, the powder 70 is discharged from the support cylinder 152 through the hole 179a while the base structure 178 is inserted into the discharge container 140. The powder 70 can be easily replenished during the plasma processing.

A structure for taking out the powder 70 will be described.
As shown in FIGS. 20 and 28, after the plasma treatment is performed on the powder 70 while rotating the discharge vessel 140 about the substantially horizontal axis on the rotating device 5, the discharge with the electrode structure 142 still inserted. The container 140 is erected with its opening 140a facing upward.

  Subsequently, after removing the fixture 149 that sandwiches and fixes the disk 179 of the electrode structure 142 and the flange portion 140a1 of the discharge vessel 140, the axial side edge portion 144c of the stirring blade 144 is connected to the inner wall 140b of the discharge vessel 140. , The electrode structure 142 is raised and taken out from the opening 140 a and is detached from the discharge vessel 140.

  As a result, only the powder 70 remains in the discharge vessel 140 simply by detaching the electrode structure 142 configured separately from the discharge vessel 140 after the plasma treatment. . For this reason, only the discharge vessel 140 can be handled, the powder 70 after the treatment can be easily collected, and the deposits in the discharge vessel 140 can be easily removed, so that the processing time required for the entire plasma treatment can be reduced. Shortening and further improvement of maintainability can be achieved.

  Next, the results of investigation on the arrangement of the discharge rods 6 suitable for glow discharge will be described with reference to FIGS. 10, 11, 29, and 30. FIG.

[Processing method]
As shown in FIGS. 10 and 11, using the above-described plasma processing apparatus 1D, in the discharge vessel 3A, an average particle size of 300 μm, 1 kg of polypropylene powder (manufactured by Nippon Polypro Co., Ltd., NOVATEC P8000S, hereinafter referred to as “powder”) ) Is enclosed (encapsulation process). At this time, according to the surface treatment or surface modification applied to the powder, the discharge rod 6 is removed from the support structure 71 to change the type of the glass tube 6b, or the powder is put into the discharge vessel 3A together with the powder as a separate agent. can do. The rod-shaped electrode 6a of the discharge rod 6 in the discharge vessel 3A is formed of a stainless steel wire (diameter 1.6 mm), and the glass tube 6b is formed of a quartz glass tube (outer diameter 4 mm, inner diameter 2 mm).

  Subsequently, a mixed gas 37 containing 20 l / min helium gas and 2 l / min nitrogen gas is filled into the discharge vessel 3A from the shaft pipe 25 to form an inert gas atmosphere, and the discharge vessel 3A is rotated substantially horizontally. A 15 kHz sine wave voltage is applied between the electrode unit 2 and the wire mesh 4 by the AC power source 23 while rotating within a rotational speed range of 5 to 8 rpm after being mounted on the device 5, and a predetermined plasma output of 100 to 2000 W is applied. Time plasma treatment was performed (processing step).

[Observation method]
As shown in FIG. 29, in the electrode unit 2, the circumferential interval y between the adjacent glass tubes 6b and the radial interval x between the glass tube 6b and the inner wall 12Ab of the glass container body 12A are changed. The discharge state of glow discharge was observed, and at the same time, the fluidity of the powder flowing in the discharge vessel 3A was also observed.

  Specifically, both the discharge state and the fluidity are visually observed from the outside, and the discharge state among them is because the discharge of the glow discharge in each discharge rod 6 is stable and the overlapping of the irradiation regions 135 is large. When the plasma density is sufficient, there is no uneven emission, and the emission intensity is high (emission intensity is large), the discharge is stable, but since the overlap of the irradiated region 135 is small, no emission unevenness occurs but the emission intensity is high. When it is small (no light emission unevenness), the discharge is unstable, or the irradiation areas 135 do not overlap at all, so that the plasma density becomes insufficient, and light emission unevenness occurs (light emission unevenness).

  When the powder flows smoothly in any of the circumferential gap 137 between the adjacent glass tubes 6b and the radial gap 136 between the glass tubes 6b and the container body 12A (excellent), the fluidity is such that the radial gap 136, If the powder flows in any of the circumferential gaps 137, but at least one of the powder stagnation is good (good), powder clogging occurs in at least one of the radial gap 136 and the circumferential gap 137 and the flow is hindered. The cases were classified into three stages (bad).

[Observation results]
As shown in FIG. 30, there is no light emission unevenness and the powder fluidity is good when both the radial interval x and the circumferential interval y are in the range of 2 to 20 mm. This is because when the radial interval x is less than 2 mm, the flow resistance when the powder passes through the radial gap 136 increases, and the flow of the powder in the discharge region 45 is inhibited, while the radial interval x is 20 mm. Exceeds the distance between the discharge rod 6 and the wire mesh 4, and the voltage required for the discharge between the two electrodes also increases, so that it is easy to shift to arc discharge and the glow discharge is unstable. It is thought to be.

  Further, when the circumferential interval y is less than 2 mm, the flow resistance when the powder passes through the circumferential gap 137 between the adjacent glass tubes 6b increases, and the flow of the powder between the inside and outside of the electrode unit 2 is hindered. If the circumferential distance y exceeds 20 mm, the overlapping portion of the glow discharge irradiation areas 135 by the adjacent discharge rods 6 becomes small, and the plasma density becomes insufficient.

  That is, while sufficiently securing gaps 136 and 137 necessary for the flow of powder around the discharge rod 6, the radial interval x is appropriately limited so as to shift from glow discharge to arc discharge by applying a high voltage. In addition to being suppressed, the circumferential interval y was appropriately limited, and it was possible to optimize the overlapping state of the discharge areas of the glow discharge by the adjacent discharge rods.

  More preferably, the radial interval x is set to 5 to 15 mm and the circumferential interval y is set to 6 to 15 mm. In this range, there is no uneven emission, and the emission intensity is high, and the powder can be smoothly flowed without stagnation.

  Next, the results of performing the plasma treatment under the above-described proper arrangement conditions of the discharge rod 6 will be described with reference to Table 1.

[Processing method]
In the above-described plasma processing apparatus 1D in which 42 discharge rods 6 are arranged at appropriate intervals (radial interval x = 10 mm, circumferential interval y = 6 mm), the powder ( After enclosing the average particle diameter of 300 μm, 1 kg), the discharge vessel 3A filled with a mixed gas 37 containing helium gas (20 l / min) and nitrogen gas (2 l / min) to make an inert gas atmosphere is rotated (5- The plasma treatment was performed for 5 minutes with an AC power source 23 (15 kHz, 1000 W).

[Analysis method]
The depth number of the powder as obtained (hereinafter referred to as “untreated powder”) and the powder (hereinafter referred to as “treated powder”) obtained by subjecting this untreated powder to plasma treatment by the above-described processing method. The surface layer part of nm was analyzed with an X-ray photoelectron spectrometer (manufactured by Shimadzu Corporation, ESCA3400).

[result of analysis]
Table 1 shows the results of comparing the nitrogen / carbon atomic ratio N / C and the oxygen / carbon atomic ratio O / C calculated from the XPS spectrum of the powder between the untreated powder and the treated powder. .

  According to Table 1, for N / C, what was not detected in the untreated powder became detected in the treated powder, and for O / C, the treated powder increased about 10 times that of the untreated powder. ing.

  That is, by performing an appropriate plasma treatment using the plasma treatment apparatus of the present invention, both the nitrogen functional group and the oxygen functional group could be normally added to the powder surface.

  As described above, the plasma apparatus to which the present invention is applied and the method thereof are compact, but the processing amount per process object such as powder is greatly increased, and the processing time is also short. .

1, 1A, 1B, 1C, 1D, 1F Plasma treatment apparatus 2, 2A Electrode unit 3, 3A, 140 Discharge vessel 4 Wire mesh (external electrode body)
5 Rotating device 6, 6A, 26 Discharge rod 6a, 26a Rod electrode 6b, 26b Glass tube (first dielectric)
21, 22 Sub-electrode unit 26A Discharge rod (cooling type discharge rod)
26B Cooling pipe (first dielectric simple substance)
45 Discharge area 47 Discharge tube (cooling type discharge tube)
48 Cylindrical electrode 49 Glass cylinder (third dielectric)
55 Cooling tube (third dielectric simple substance)
63 rake member 64 stay discharge part 64a inflow port 64b stay chamber 64c discharge port 66 rake member with hole 66b sieve discharge part 66b1 discharge hole 70 powder (processed object)
73, 77 Support member 74, 78 Mounting member 84, 85 Adjustment mechanism 140a Opening 140b Inner wall 142 Electrode structure 143 Lid unit 144 Stirring blade 144a Front end (axial end)
144c Axial side edge 179 Disc (lid)
179a hole 146 plug part 173, 174 ventilation path x radial direction interval y circumferential direction interval

Claims (16)

An electrode unit in which discharge rods formed by covering rod-shaped electrodes with a first dielectric are arranged in parallel to each other in an annular shape at predetermined circumferential intervals;
A cylindrical discharge vessel disposed outside the electrode unit, in which an object to be processed is enclosed, and having a second dielectric;
An external electrode body disposed outside the discharge vessel;
A rotating device that rotates the discharge vessel in a state where glow discharge is generated by applying an alternating current or pulse voltage between the electrode unit and the external electrode body;
A plasma processing apparatus comprising: a discharge area expansion structure capable of extending a discharge area of the glow discharge to the inside and outside of an electrode unit. The discharge rod is
In the discharge vessel, the radial interval between the first dielectric and the second dielectric and the circumferential interval between the adjacent first dielectrics are both 2 to 20 mm. The plasma processing apparatus according to claim 1. The discharge area expansion structure is:
2. A single or a plurality of sub-electrode units concentrically with the electrode unit, wherein the discharge rods are arranged in an annular shape at a predetermined circumferential interval in parallel to each other in a space inside the electrode unit. The plasma processing apparatus according to claim 2. The radially innermost sub-electrode unit in the discharge vessel is
Instead of the prescribed discharge rod,
The cooling medium has at least one of a cooling type discharge rod capable of flowing through an internal gap between the rod-shaped electrode and the first dielectric, and the first dielectric single body capable of flowing inside the cooling medium. Plasma processing equipment. A cooling type discharge cylinder disposed on the axial center in the discharge vessel and formed by a cylindrical electrode covered with a third dielectric material capable of flowing a cooling medium inside; or disposed on the axial center for cooling The plasma processing apparatus according to any one of claims 1 to 4, wherein the medium includes the third dielectric single body capable of flowing inside. The discharge area expansion structure is:
In the discharge vessel, only the end of the discharge rod is attached to the axial end surface to support the discharge rod, and a plurality of arcuate attachment members that are arranged on the same circumference and can form a ring ,
A radial support member having a plurality of branches extending radially from the axis of the ring;
The plasma processing apparatus according to any one of claims 1 to 5, further comprising an adjustment mechanism capable of changing a mounting position of the mounting member with respect to the branch portion to expand a radial interval. A rake member that rotates together with the discharge vessel and whose outer peripheral side in the centrifugal direction curves toward the rotational direction;
An inflow port on the inner peripheral side in the centrifugal direction on the front side in the rotational direction of the scooping member, a staying chamber communicating with the inflow port, and communicating with the staying chamber and on the outer peripheral side in the centrifugal direction with respect to the staying chamber, from the inlet Has a small area outlet,
The scooped up object to be processed includes a stirring blade having a staying discharge portion that gradually flows down from the inflow port to a discharge region through a staying chamber in the middle of the discharge port. The plasma processing apparatus according to claim 6. Rotating together with the discharge vessel, the outer peripheral side in the centrifugal direction is curved in the rotational direction, and the sieve discharge part having a discharge hole in the rotational direction has a rake member with a hole disposed on the outer peripheral side in the centrifugal direction. The plasma processing apparatus according to any one of claims 1 to 6. The electrode unit;
A lid unit for closing the opening of the discharge vessel and supporting the electrode unit;
The electrode unit is interposed between adjacent discharge rods, the axial end is fixed to the lid unit, and the axial side edge is slidably abutted on and supported by the inner wall of the discharge vessel. Agitated blades,
The plasma processing apparatus according to any one of claims 1 to 8, comprising an electrode structure integrally incorporated. The lid unit is
The plasma according to claim 9, further comprising a plug portion that is detachably mounted in a hole formed in the lid that closes the opening, and in which a current path and a ventilation path for the glow discharge are integrated. Processing equipment. Disposing the discharge rods formed by covering the rod-shaped electrodes with the first dielectric in parallel with each other and arranging the electrode units in an annular shape at predetermined circumferential intervals on the inside, the external electrode body on the outside, A sealing step in which a cylindrical discharge vessel having a second dielectric is interposed between the electrode unit and the external electrode body, and an object to be processed is enclosed in the discharge vessel;
A discharge vessel with an inert gas atmosphere inside is rotated by a rotating device, and an alternating current or pulse voltage is applied between the electrode unit and the external electrode body to generate glow discharge, thereby providing a discharge area expansion structure. And a processing step of performing plasma processing by flowing the object to be processed in a discharge region of glow discharge extended to the inside and outside of the electrode unit. The discharge rod is
In the discharge vessel, the radial interval between the first dielectric and the second dielectric and the circumferential interval between the adjacent first dielectrics are both 2 to 20 mm. The plasma processing method according to claim 11. The discharge area expansion structure is:
The sub-electrode unit in which the discharge rods are arranged in an annular shape at a predetermined circumferential interval in parallel to each other in a space inside the electrode unit is single or plural concentrically with the electrode unit. The plasma processing method according to claim 12. The radially innermost sub-electrode unit in the discharge vessel is
Instead of the prescribed discharge rod,
The cooling medium has at least one of a cooling type discharge rod capable of flowing through an internal gap between the rod-shaped electrode and the first dielectric, and the first dielectric single body capable of flowing inside the cooling medium. Plasma processing method. A cooling type discharge cylinder disposed on the axial center in the discharge vessel and formed by a cylindrical electrode covered with a third dielectric material capable of flowing a cooling medium inside; or disposed on the axial center for cooling The plasma processing method according to any one of claims 11 to 14, wherein the medium includes the third dielectric simple substance capable of flowing inside. The discharge area expansion structure is:
In the discharge vessel, only the end of the discharge rod is attached to the axial end surface to support the discharge rod, and a plurality of arcuate attachment members that are arranged on the same circumference and can form a ring ,
A radial support member having a plurality of branches extending radially from the axis of the ring;
The plasma processing method according to any one of claims 11 to 15, further comprising an adjustment mechanism capable of changing a mounting position of the mounting member with respect to the branch portion to expand a radial interval.

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