Mixing and defoaming equipment and production method

Abstract

To provide an agitation / defoaming processor which makes user-friendliness satisfactory, and has high agitation performance and defoaming performance.SOLUTION: An agitation / defoaming processor 100 includes a container 1 for storing a processed object 5 therein, a container holder 106 mounted with the container 1, and a driving mechanism D for rotating the container holder 106 around a rotation shaft center and revolving the rotation shaft center, and includes a plasma guide part 10 for guiding gas containing plasma to the inside of the container 1.SELECTED DRAWING: Figure 1

Description

[Technical Field]

[0001] The present disclosure relates to an agitation and degassing treatment device that includes a container that accommodates an object to be treated inside, a container holder on which the container is mounted, and a drive mechanism that rotates the container holder about its rotation axis and revolves around the rotation axis, as well as a production method for producing an object to be treated that has been agitated and / or degassed. [Background technology]

[0002] In recent years, various fine particles, including nanoparticles, have been used to manufacture articles. Such fine particles often have large surface energies, resulting in aggregation of fine primary particles into large secondary particles. When manufacturing articles, it is necessary to break down the aggregated secondary particles to return them to the primary particle state.

[0003] Examples of devices for stirring the material to be treated to improve dispersibility include a magnetic stirrer, an ultrasonic homogenizer, a high-speed homomixer, a bead mill, and a planetary mixer.

[0004] However, conventional devices may not be able to sufficiently break down agglomerated secondary particles into primary particles, or the fine particles may re-aggregate after the treatment, even if they are dispersed in the liquid during the stirring treatment.

[0005] As another technique, Patent Document 1 (Japanese Patent No. 6510903) describes a method for dispersing powder in a dispersion medium, in which plasma is generated to increase the zeta potential around powder having alumina on the surface, thereby dispersing the powder well in the dispersion medium. [Prior art documents] [Patent documents]

[0006] [Patent Document 1] Patent No. 6510903 Summary of the Invention [Problem to be solved by the invention]

[0007] The method described in Patent Document 1 involves immersing an electrode for generating plasma in the dispersion medium, which poses several problems. For example, the electrode may be damaged by discharge and may become mixed into the dispersion medium. Another problem is that the heat generated by the electrode may heat the dispersion medium. Furthermore, because the electrode comes into direct contact with the dispersion medium, it is necessary to select an electrode material that does not chemically react with the dispersion medium. Furthermore, if the dispersion medium contains a highly flammable liquid such as an organic solvent, it may ignite during plasma generation. Furthermore, an electrolyte must be added to the dispersion medium to generate plasma.

[0008] As described above, conventional processing devices are not easy to use.

[0009] The present disclosure has been made in view of the above-mentioned problems, and its purpose is to provide an agitation / defoaming treatment device and a production method thereof that are easy to use and have high agitation and defoaming performances. [Means for solving the problem]

[0010] The configuration of the stirring and degassing treatment device according to one embodiment of the present disclosure is as follows: A stirring and degassing treatment apparatus includes a container for accommodating an object to be treated therein, a container holder on which the container is mounted, and a drive mechanism for rotating the container holder about its rotation axis and revolving the rotation axis, and further includes a plasma induction unit for guiding a gas containing plasma into the container. 、 The container includes a cylindrical main body having a bottom and an opening at an upper end, and a lid removably attached to the opening of the main body, a part of the plasma guide portion is inserted into the container through a central portion of the lid; The lid has an exhaust vent formed at a position closer to the center than to the end of the lid. . Here, the container may be provided with a plasma generating unit that is provided outside the container and generates plasma, and the plasma guiding unit may be configured to guide a gas containing the plasma generated by the plasma generating unit into the container. In addition, the plasma induction unit may be configured to include a rotation unit that is attached to the container and can rotate in synchronization with the rotation of the container holder, an orbital unit that can rotate in synchronization with the revolution of the container holder, and a rotary connector that connects the rotation unit and the orbital unit, and to guide gas containing plasma generated in the plasma generation unit into the inside of the container via the orbital unit, the rotary connector, and the rotation unit.

[0011] According to the above configuration, a container containing the workpiece is mounted on the container holder, and the drive mechanism can be operated while the plasma guider introduces plasma-containing gas into the container. In other words, by performing plasma treatment on the workpiece while stirring and degassing the workpiece, active species such as radicals generated by the plasma action can be expected to enhance the dispersion effect of particles and fibers contained in the workpiece. Therefore, even if particles and fibers aggregate, they can be broken down or defibrated, and their re-aggregation can be suppressed. Additionally, the plasma irradiation is performed while the workpiece is flowing by rotating and revolving the container, which has the advantage of evenly applying the plasma action to the workpiece. Furthermore, the rotation and revolution of the container enhances the plasma action due to the heat generated in the workpiece, which is expected to enhance the dispersion effect of particles and fibers contained in the workpiece.

[0012] Furthermore, as particles and fibers contained in the material to be treated become more aggregated, their size increases, which can make the material more susceptible to entraining air and generating bubbles during the agitation and degassing process. However, with this configuration, it is expected that the particles and fibers contained in the material to be treated will be crushed or defibrated, reducing their size. Therefore, the material to be treated may be less likely to entrain air during the agitation and degassing process, which may make it more difficult for bubbles to be generated.

[0013] Furthermore, since there is no need to bring the electrodes for generating plasma into contact with the workpiece, the electrode material does not get mixed into the workpiece, the workpiece is not heated by the heat generated by the electrodes, and the electrodes do not chemically react with the workpiece, resulting in a user-friendly mixing and degassing treatment device.

[0015] In addition, According to the above configuration, the plasma-containing gas flowing into the container flows from the center of the lid toward the workpiece, spreads on the surface of the workpiece, rises along the inner wall of the main body, and circulates inside the container while changing direction near the end of the lid. After circulating along this path, a portion of the gas is discharged to the outside of the container through the vent. In other words, the vent is provided at a location where the gas reaches after being supplied to the inside of the container and circulating. As a result, it is expected that the discharge of the plasma-containing gas supplied into the container to the outside of the container can be delayed. In other words, the plasma flowing into the container can be given sufficient time to come into contact with the workpiece inside the container.

[0016] In still another configuration of the stirring and degassing treatment device according to the present disclosure, the plasma induction section has a nozzle inserted into the container and emitting a gas containing plasma.

[0017] According to the above configuration, by changing the shape of the nozzle, it is possible to freely change the direction in which the plasma-containing gas is irradiated onto the workpiece.

[0018] In still another configuration of the agitation / defoaming treatment device according to the present disclosure, the nozzle is installed at a position where it does not come into contact with the object to be treated.

[0019] According to the above configuration, the nozzle does not come into contact with the workpiece, which prevents the workpiece from chemically reacting with the nozzle material and prevents foreign matter adhering to the nozzle from mixing into the workpiece.

[0020] A production method according to one embodiment of the present disclosure is a production method for producing a processed object that has been stirred and / or degassed using a stirring and degassing treatment device including a container that accommodates a processed object therein, a container holder on which the container is mounted, a drive mechanism that rotates the container holder about a rotation axis and revolves the container holder around the rotation axis, and a plasma induction unit that introduces a plasma-containing gas into the container. The container comprises a cylindrical main body having a bottom and an opening at an upper end, and a lid removably attached to the opening of the main body, a part of the plasma induction unit is inserted into the container through a central part of the lid, and an exhaust vent is formed in the lid at a position closer to the central part than the end of the lid, The container that houses the object to be processed is rotated and revolved, and the plasma-containing gas is supplied into the container for at least a portion of the time during the rotation and revolution.

[0021] According to the above configuration, a container containing a workpiece can be mounted on a container holder, and the drive mechanism can be operated while introducing plasma-containing gas into the container using the plasma guide. For example, if the workpiece contains particles and fibers, plasma treatment can be performed on the workpiece while stirring and degassing the workpiece. This is expected to enhance the dispersion effect of the particles and fibers contained in the workpiece due to the active species, such as radicals, generated by the plasma action. Therefore, even if particles and fibers aggregate, they can be broken down or defibrated, and their re-aggregation can be suppressed. In addition, plasma irradiation is performed while the workpiece is flowing by rotating and revolving the container, which has the advantage of evenly applying the plasma action to the workpiece. Furthermore, the rotation and revolution of the container enhances the plasma action due to the heat generated in the workpiece, which is expected to enhance the dispersion effect of particles and fibers contained in the workpiece. Therefore, a production method for producing a workpiece that is well stirred and / or degassed can be realized. In addition, with the above configuration, the plasma-containing gas flowing into the container flows from the center of the lid toward the workpiece, spreads on the surface of the workpiece, rises along the inner wall of the main body, and circulates inside the container while changing direction near the end of the lid. After circulating along this path, a portion of the gas is discharged to the outside of the container through the vent. In other words, the vent is provided at a location where the gas reaches after being supplied to the inside of the container and circulating. As a result, it is expected that the discharge of the plasma-containing gas supplied into the container to the outside of the container can be delayed. In other words, the plasma flowing into the container can be given sufficient time to come into contact with the workpiece inside the container. [Brief explanation of the drawings]

[0022] [Figure 1] FIG. 1 is a block diagram showing an example of an agitation and defoaming treatment device. [Figure 2] 1 is a schematic diagram illustrating an example of a plasma generating unit and a plasma directing unit. [Figure 3] FIG. 10 is a diagram showing a state in which a workpiece is irradiated with plasma inside a container. [Figure 4] 10A and 10B are diagrams showing examples of a lid for a container. [Figure 5] FIG. 2 is a diagram illustrating an example of the configuration of a nozzle. [Figure 6] FIG. 1 is a diagram showing the results of a crushing test of carbon fibers. [Figure 7] FIG. 1 is a diagram showing the results of a crushing test of carbon fibers. [Figure 8] FIG. 1 is a diagram showing the results of a crushing test of carbon fibers. [Figure 9] FIG. 1 is a diagram showing the results of a crushing test of titanium oxide. [Figure 10] FIG. 1 is a diagram showing the results of a crushing test of titanium oxide. [Figure 11] FIG. 1 is a diagram showing the results of a silica fume crushing test. DETAILED DESCRIPTION OF THE INVENTION

[0023] An agitation and defoaming treatment device 100 according to an embodiment will be described below with reference to the drawings. FIG. 1 is a block diagram illustrating an example of an agitation and degassing treatment device 100. FIG. 2 is a schematic diagram illustrating an example of a plasma generator 2 and a plasma induction unit 10. As illustrated, the agitation and degassing treatment device 100 includes a container 1 that accommodates a workpiece 5, a container holder 106 on which the container 1 is mounted, and a drive mechanism D that rotates the container holder 106 about its axis of rotation and revolves around the axis of rotation. Additionally, the agitation and degassing treatment device 100 includes a plasma induction unit 10, which is a gas passage that introduces plasma-containing gas into the container 1. While FIG. 1 illustrates an example in which two container holders 106 are provided in the agitation and degassing treatment device 100, the number of container holders 106 can be changed. For example, when one container holder 106 is provided in the agitation and degassing treatment device 100, the agitation and degassing treatment device 100 may include a weight for balancing during rotation.

[0024] The drive mechanism D of this embodiment shown in Figure 1 includes a revolving gear 101, a rotating drum 102, a revolving shaft 103, a drive motor 104, a revolving table 105, a rotating gear 108, an intermediate gear 109, a sun gear 110, a gear 111, a gear 112, and a gear 113.

[0025] In the drive mechanism D, a rotating drum 102 having a revolving gear 101 is rotatably supported via a bearing on a fixed shaft, i.e., a revolution shaft 103. Rotational motion by a drive motor 104 is transmitted to the rotating drum 102 via the revolving gear 101, causing the rotating drum 102 to rotate around the revolution axis X2 of the revolution shaft 103. A revolution table 105 is fixedly connected to the rotating drum 102 and rotates together with the rotating drum 102. A container holder 106 is supported on the revolution table 105 so as to be rotatable around its own rotation axis X1. Therefore, the container holder 106 rotates, i.e., revolves, around the revolution axis X2 of the revolution shaft 103 due to the rotation of the revolution table 105.

[0026] The container holder 106 is connected to the rotating gear 108 so as to rotate together with the rotating gear 108. The rotating gear 108 meshes with an intermediate gear 109 that is rotatably supported on the revolution table 105 via a bearing. The intermediate gear 109 meshes with a sun gear 110. The sun gear 110 is disposed outside the rotating drum 102 and is rotatably supported relative to the rotating drum 102 via a bearing.

[0027] The sun gear 110 meshes with a gear 111. A braking force of a braking device 114 such as a powder brake is transmitted to the gear 111 via gears 112 and 113 which mesh with each other.

[0028] When no braking force is applied by the brake device 114, that is, when the braking force is zero, the sun gear 110 rotates in accordance with the rotation of the rotating drum 102.

[0029] When the braking force of brake device 114 is transmitted to sun gear 110 via gear 111, the rotational speed of sun gear 110 decreases compared to the rotational speed of rotating drum 102, causing a difference between the rotational speed of sun gear 110 and the rotational speed of revolution table 105 connected to rotating drum 102. As a result, intermediate gear 109 rotates relative to sun gear 110. Because intermediate gear 109 meshes with rotation gear 108, rotation gear 108 rotates, and container holder 106 rotates about rotation axis X1, i.e., rotates on its axis.

[0030] The above-described agitation and degassing treatment device 100 is an example of a configuration in which the container holder 106 is revolved and rotated on its axis by a single drive motor 104, but the configuration of the agitation and degassing treatment device 100 is not limited to the example shown in FIG. 1. For example, the agitation and degassing treatment device 100 may be provided with separate drive motors for revolution and rotation to revolve the container holder 106 on its axis, or may have other configurations. The rotational speeds of the rotation and revolution of the container 106 in the agitation and degassing treatment device 100 can be set as appropriate.

[0031] The stirring and degassing treatment device 100 is provided outside the vessel 1 and includes a plasma generating unit 2 that generates plasma. The plasma generating unit 2 includes a voltage applying unit 2a having a pair of electrodes that generates plasma, and a power supply unit 2b that applies a voltage between the pair of electrodes of the voltage applying unit 2a. A gas is supplied to the plasma generating unit 2 from a gas supply source 3. For example, nitrogen gas, argon gas, etc. are supplied from the gas supply source 3. The gas supplied from the gas supply source 3 is then supplied to the voltage applying unit 2a, where it is converted into a plasma state. The gas supplied from the gas supply source 3 serves as a carrier gas for the plasma generated in the voltage applying unit 2a of the plasma generating unit 2, and sends the generated plasma to the plasma leading unit 10.

[0032] The plasma guiding unit 10 guides the gas containing plasma generated in the plasma generating unit 2 into the interior of the container 1. In the example shown in FIG. 2, the plasma guiding unit 10 includes a rotation unit 15 attached to the container 1 and rotatable in synchronization with the rotation of the container holder 106, a revolution unit 13 rotatable in synchronization with the revolution of the container holder 106, and a rotary connector 14 connecting the rotation unit 15 and the revolution unit 13. The gas containing plasma generated in the plasma generating unit 2 is guided into the interior of the container 1 via the revolution unit 13, the rotary connector 14, and the rotation unit 15. In addition, the plasma guiding unit 10 includes a fixed unit 11 that does not rotate or revolve around its axis, and a rotary connector 12 connecting the fixed unit 11 and the revolution unit 13. That is, the gas containing plasma generated in the plasma generating unit 2 is guided into the interior of the container 1 via the fixed unit 11, the rotary connector 12, the revolution unit 13, the rotary connector 14, and the rotation unit 15.

[0033] The agitation and degassing treatment device 100 further includes a control unit 4 that controls each unit of the agitation and degassing treatment device 100 and the gas supply source 3. Under the control of the control unit 4, the agitation and degassing treatment device 100 and the gas supply source 3 rotate and revolve the container 1 attached to the container holder 106, thereby supplying gas to the container 1. The control unit 4 includes, for example, a processor circuit and a recording medium such as a hard disk or memory on which a program is recorded, and executes control processing according to the program stored in the recording medium.

[0034] FIG. 3 shows how the workpiece 5 is irradiated with plasma inside the vessel 1. FIG. 4 shows the configuration of the lid 1b of the vessel 1. The vessel 1 includes a cylindrical body 1a with a bottom and an opening at the top, and a lid 1b that is detachably attached to the opening of the body 1a. In the illustrated example, the cross-section of the body 1a is circular. That is, one end of the body 1a along the central axis of the cylinder is closed to form the bottom, and the other end is open to form the opening. The opening of the body 1a and the lid 1b are also circular. A portion of the plasma induction unit 10 penetrates the center of the lid 1b and is inserted into the vessel 1. The portion of the plasma induction unit 10 inserted into the vessel 1 has a nozzle 15a inserted into the vessel 1 and emitting a plasma-containing gas. The nozzle 15a is part of the rotation unit 15 and is installed in a position that does not contact the workpiece 5. The plasma-containing gas emitted from the nozzle 15a hits the surface of the object 5 being stirred and degassed.

[0035] The control unit 4 controls the drive mechanism D and a valve provided in the plasma induction unit 10 to rotate and revolve the container 1 containing the workpiece 5 therein, and supplies plasma-containing gas into the container 1 for at least a portion of the rotation and revolution. This realizes a production method for producing the workpiece 5 that has been stirred and / or degassed using the stirring and degassing treatment device 100. In detail, the control unit 4 causes the actuator to open the valve and continuously supply plasma-containing gas from the plasma generation unit 2 to the container 1 all or part of the time while the drive mechanism D simultaneously rotates and revolves the container 1 to perform the stirring and degassing treatment of the workpiece 5. The control unit 4 may further cause the plasma generation unit 2 to supply plasma-containing gas to the container 1 before and / or after the stirring and degassing treatment of the workpiece 5 by simultaneously rotating and revolving the container 1.

[0036] An exhaust vent hole 1c is formed in the lid 1b at a position closer to the center than the end of the lid 1b. Gas can move between the inside and outside of the container 1 via this vent hole 1c. In this embodiment, while plasma-containing gas is continuously supplied to the inside of the container 1, the gas inside the container 1 is continuously exhausted to the outside of the container 1 via the vent hole 1c.

[0037] As shown in FIG. 3, the plasma-containing gas is emitted from the lid 1b toward the bottom of the main body 1a. The vent 1c is formed in the lid 1b. In the illustrated example, the two vents 1c are positioned closer to the center of the lid 1b than to the ends, sandwiching the nozzle 15a between them. That is, the nozzle 15a is positioned at the center of the circular lid 1b, and each vent 1c is positioned closer to the center of the lid 1b than to the radially outer ends of the circular lid 1b. As a result, as shown by the arrows in FIG. 3, the plasma-containing gas supplied to the interior of the container 1 hits the workpiece 5, rises along the inner wall of the main body 1a, changes direction near the end of the lid 1b, circulates within the container 1, and is then discharged to the outside of the container 1 through the vent 1c formed in the lid 1b. In this way, the vent 1c is located at the location where the gas reaches after being supplied and circulated inside the container 1. As a result, it is expected that the discharge of the plasma-containing gas supplied into the container 1 to the outside of the container 1 can be delayed. In other words, there is an advantage in that the contact time between the plasma and the object 5 to be treated is extended.

[0038] FIG. 5 illustrates an exemplary configuration of a nozzle 15a. FIG. 5(a) illustrates a nozzle in which gas is emitted from the tip of the nozzle 15a in a linear fashion parallel to the central axis of the nozzle 15a and in a direction away from the central axis of the nozzle 15a. FIG. 5(b) illustrates a nozzle in which a relatively large amount of gas is emitted from the tip of the nozzle 15a in a linear fashion parallel to the central axis of the nozzle 15a, and a relatively small amount of gas is emitted around the tip in a linear fashion parallel to the central axis of the nozzle 15a. FIG. 5(c) illustrates a nozzle in which all gas is emitted from the tip of the nozzle 15a in a linear fashion parallel to the central axis of the nozzle 15a. FIG. 5(d) illustrates a nozzle in which approximately the same amount of gas is emitted from the tip of the nozzle 15a in a direction parallel to the central axis of the nozzle 15a and in a direction away from the central axis of the nozzle 15a. The nozzle 15a in FIG. 5(d) emits gas over a wider area than the nozzle 15a in FIG. 15(a). In this way, the direction and amount of gas emitted from the nozzle 15a can be set appropriately.

[0039] Next, the effect of performing the stirring and degassing process while irradiating the workpiece 5 with plasma will be described.

[0040] (1) Test 1: Crushing test of carbon fiber (0.3 g) The stirring and degassing conditions were as follows: Material 5: 0.3 g of carbon fiber, 50 g of water Orbital rotation speed: 1000 rpm Rotation speed: 1000 rpm Time: 600 seconds

[0041] The carbon fiber used was KUREKA CHOP KGF-200, available from KUREHA CORPORATION. The grade of KUREKA CHOP is M-2007S, and the diameter of the carbon fiber is 14.5 μm.

[0042] The plasma irradiation conditions are as follows: The plasma generator 2 was a tube inner wall atmospheric pressure plasma generator S5000-T manufactured by Sakigake Semiconductor Co., Ltd. The power supply was single-phase 100V (60Hz), 10A. Nitrogen gas was supplied from the gas supply source 3 to the plasma generator 2 at a gas pressure of 0.3MPa and a gas flow rate of 30L / min. The "HV TIMER" control on the tube inner wall atmospheric pressure plasma generator S5000-T was set to 9999 seconds, and the "power adjustment" control was set to 100. In addition, at the start of the disintegration test, the switch on the tube inner wall atmospheric pressure plasma generator S5000-T was manually operated when the revolution speed reached 1000 rpm, to start the gas supply and plasma irradiation in tandem. At the end of the disintegration test, the switch on the tube inner wall atmospheric pressure plasma generator S5000-T was manually operated when deceleration began, to stop the gas supply and plasma irradiation in tandem. The nozzle 15a used was the type shown in FIG. 5(a).

[0043] FIG. 6 shows the results of a carbon fiber disintegration test. Specifically, FIG. 6 shows images of carbon fibers contained in the object to be treated 5 observed with an optical microscope after performing the agitation and degassing treatment in the agitation and degassing treatment device 100 while irradiating plasma under the above-mentioned conditions, after performing the agitation and degassing treatment in the agitation and degassing treatment device 100 without irradiating plasma, and after agitating the object to be treated 5 by hand-shaking the container 1 for 10 seconds without irradiating plasma, i.e., by "manual mixing." The magnifications are 200x and 500x. As shown in the figure, without plasma irradiation, multiple carbon fibers remain aggregated. In contrast, with plasma irradiation, it can be seen that the multiple carbon fibers are well disintegrated.

[0044] Figure 7 shows the results of a carbon fiber disintegration test. Specifically, Figure 7 shows the results of pulse NMR measurements of the treated material 5 after performing the stirring and degassing treatment in the stirring and degassing treatment device 100 while irradiating plasma under the above conditions, after performing the stirring and degassing treatment in the stirring and degassing treatment device 100 without plasma irradiation, and after agitating the treated material 5 by "manual mixing" (shaking the container 1 by hand for 10 seconds) without plasma irradiation. The higher the Rsp value shown on the vertical axis, the higher the dispersibility of the particles in water. This pulse NMR was measured using a MagnoMeter XRS (available from Majestic Japan Co., Ltd.). As shown in the figure, the Rsp value was lowest when the treated material 5 was agitated by "manual mixing." The Rsp value was highest when the agitation and degassing treatment was performed while irradiating plasma. The Rsp value was highest, indicating the highest dispersibility of the carbon fiber. In contrast, when stirring and degassing treatment was performed without plasma irradiation, the Rsp value was larger than that of "hand mixing," meaning that dispersibility was improved, but the dispersibility of the carbon fiber remained low compared to when plasma irradiation was performed.

[0045] (2) Test 2: Crushing test of carbon fiber (2 g) The stirring and degassing conditions were as follows: Material 5: 2g of carbon fiber, 50g of water Orbital rotation speed: 1000 rpm Rotation speed: 1000 rpm Time: 1800 seconds

[0046] The carbon fiber used was KUREKA CHOP KGF-200, available from KUREHA CORPORATION. The grade of KUREKA CHOP is M-2007S, and the diameter of the carbon fiber is 14.5 μm.

[0047] Fig. 8 shows the results of a carbon fiber crushing test. Specifically, Fig. 8 shows images of the object 5 observed after the agitation and degassing treatment was performed in the agitation and degassing treatment device 100 while irradiating plasma under the same conditions as in Experiment 1 above, and after the agitation and degassing treatment was performed in the agitation and degassing treatment device 100 without irradiating plasma. After the agitation and degassing treatment was completed, the object 5 was transferred to a transparent bottle with a lid, separate from the container 1 used in the agitation and degassing treatment. Photographs were then taken of the changes in the state of the object 5 over time, from immediately after the treatment until 10 minutes later.

[0048] As is clear from Figure 8, when plasma irradiation was not performed, significant precipitation of carbon fibers was already evident after one minute. Furthermore, the precipitation of carbon fibers continued to progress rapidly thereafter. This is thought to be because the carbon fibers were not sufficiently disintegrated and remained as large aggregates. In contrast, when plasma irradiation was performed, almost no precipitation of carbon fibers was evident after one minute. Then, the precipitation of carbon fibers progressed slowly over time. In addition, when plasma irradiation was not performed, it can be seen that many carbon fibers were floating on the surface of the workpiece 5, i.e., on the surface of the water, and that many carbon fibers that were not dispersed in the water were present on the surface of the water.

[0049] (3) Test 3: Crushing test of titanium oxide (0.3 g) The stirring and degassing conditions were as follows: Material to be treated 5: 0.3 g of titanium oxide, 100 g of water Orbital rotation speed: 1000 rpm Rotation speed: 1000 rpm Time: 300 seconds

[0050] The titanium oxide used was STR-100N, sold by Sakai Chemical Industry Co., Ltd. The primary particle diameter of STR-100N measured by X-ray was 16 nm, and the specific surface area was 100 m 2 / g.

[0051] FIG. 9 shows the results of a titanium oxide disintegration test. Specifically, FIG. 9 shows images of titanium oxide contained in the workpiece 5 observed with an optical microscope after the agitation and degassing treatment was performed in the agitation and degassing treatment device 100 while irradiating plasma under the same conditions as in Experiment 1 above, and after the agitation and degassing treatment was performed in the agitation and degassing treatment device 100 without irradiating plasma. The magnifications were 200x, 500x, and 1000x. As shown in the figure, regardless of the magnification, when plasma irradiation was not performed, the titanium oxide remained aggregated. In contrast, when plasma irradiation was performed, the titanium oxide was disintegrated.

[0052] (4) Test 4: Crushing test of titanium oxide (10 g) The stirring and degassing conditions were as follows: Material to be treated 5: 10g of titanium oxide, 50g of water Orbital rotation speed: 1200 rpm Rotation speed: 1200 rpm Time: 300 seconds The titanium oxide used was STR-100N, sold by Sakai Chemical Industry Co., Ltd. The primary particle diameter of STR-100N measured by X-ray was 16 nm, and the specific surface area was 100 m 2 / g.

[0053] Figure 10 shows the results of a titanium oxide disintegration test. Specifically, Figure 10 shows the results of pulse NMR measurements of the treated material 5 after performing the agitation and degassing treatment in the agitation and degassing treatment device 100 while irradiating plasma under the same conditions as in Experiment 1 above, after performing the agitation and degassing treatment in the agitation and degassing treatment device 100 without plasma irradiation, and after agitating the treated material 5 by hand (shaking the container 1 for 10 seconds). The higher the Rsp value shown on the vertical axis, the higher the dispersibility of the particles in water. This pulse NMR was measured using a MagnoMeter XRS (available from Majestic Japan Co., Ltd.). As shown in the figure, the Rsp value was lowest when the treated material 5 was agitated by hand mixing. The Rsp value was highest when the agitation and degassing treatment was performed while irradiating plasma, indicating the highest dispersibility of titanium oxide. In contrast, when stirring and degassing treatment was performed without plasma irradiation, the Rsp value was larger than when mixed by hand, meaning that dispersibility was improved, but the dispersibility of titanium oxide remained low compared to when plasma irradiation was performed.

[0054] (5) Test 5: Silica fume crushing test The stirring and degassing conditions were as follows: Material to be treated 5: Silica fume 20g, water 30g Orbital rotation speed: 1200 rpm Rotation speed: 1200 rpm Time: 300 seconds The silica fume used was SN-5, available from Keiwa Fine Materials Co., Ltd.

[0055] Figure 11 shows the results of a silica fume crushing test. Specifically, Figure 11 shows the results of pulse NMR measurements of the treated material 5 after performing the stirring and degassing treatment in the stirring and degassing treatment device 100 while irradiating plasma under the same conditions as in Experiment 1 above, after performing the stirring and degassing treatment in the stirring and degassing treatment device 100 without plasma irradiation, and after agitating the treated material 5 by hand (shaking the container 1 for 10 seconds). The higher the Rsp value shown on the vertical axis, the higher the dispersibility of the particles in water. This pulse NMR was measured using a MagnoMeter XRS (available from Majestic Japan Co., Ltd.). As shown in the figure, the Rsp value was lowest when the treated material 5 was agitated by hand mixing. The Rsp value was highest when the agitation and degassing treatment was performed while irradiating plasma. This indicated that the dispersibility of the silica fume was maximized. In contrast, when stirring and degassing treatment was performed without plasma irradiation, the Rsp value was larger than when mixed by hand, meaning that dispersibility was improved, but the dispersibility of silica fume remained low compared to when plasma irradiation was performed.

[0056] As described above, the stirring and defoaming treatment device 100 of this embodiment can operate the drive mechanism D while mounting the container 1 containing the workpiece 5 on the container holder 106 and guiding plasma-containing gas into the container 1 using the plasma guide unit 10. In other words, by performing plasma treatment on the workpiece 5 while stirring and defoaming the workpiece 5, active species such as radicals generated by the plasma action can be expected to enhance the dispersion effect of particles, fibers, etc. contained in the workpiece 5. Furthermore, for example, the hydrophilicity of the particles, fibers, etc. is increased, which allows the particles, fibers, etc. to blend with the liquid, thereby replacing bubbles contained in aggregates of particles, fibers, etc. with the liquid, further improving the dispersibility of the particles, fibers, etc. Therefore, even if particles, fibers, etc. aggregate, they can be disintegrated or defibrated, and their re-aggregation can be suppressed. Additionally, plasma irradiation is performed while the workpiece 5 is flowing by rotating and revolving the container 1, which has the advantage of evenly applying the plasma action to the workpiece 5. Furthermore, by rotating and revolving the container 1, the action of the plasma is strengthened by the heat generated in the object 5 to be treated, which is expected to improve the dispersion effect of particles, fibers, etc. contained in the object 5 to be treated.

[0057] As particles, fibers, and the like contained in the object 5 become more aggregated, their size increases, making the object 5 more likely to entrain air and generate bubbles during the agitation and degassing treatment. However, in the agitation and degassing treatment device 100 of this embodiment, it is expected that the particles, fibers, and the like contained in the object 5 will be crushed or defibrated, reducing their size. Therefore, the object 5 will be less likely to entrain air during the agitation and degassing treatment, making it less likely to generate bubbles.

[0058] Furthermore, since there is no need to bring the electrodes of the voltage application unit 2a into contact with the workpiece 5, the material of the electrodes will not be mixed into the workpiece 5, the workpiece 5 will not be heated by the heat generated by the electrodes, and the electrode material will not chemically react with the workpiece 5, thereby realizing an easy-to-use agitation and degassing treatment device 100.

[0059] <Another embodiment> <1> In the above embodiment, the configuration of the stirring / defoaming treatment device 100 has been described using a specific example, but the configuration can be changed as appropriate. For example, in the above embodiment, an example has been described in which the plasma generating unit 2 is mounted on the stirring and degassing treatment device 100, but the plasma generating unit 2 may also be provided outside the stirring and degassing treatment device 100.

[0060] <2> In the above embodiment, several materials are exemplified as the object to be processed 5, but the type of object to be processed 5 is not limited to the above-mentioned materials, and various materials can be used.

[0061] <3> In the above embodiment, an example has been described in which plasma is generated by supplying nitrogen gas from the gas supply source 3 to the plasma generating unit 2, but the type of gas supplied from the gas supply source 3 to the plasma generating unit 2 can be changed as appropriate. For example, plasma can also be generated by supplying gas such as oxygen gas or argon gas from the gas supply source 3 to the plasma generating unit 2. In addition, it is also possible to use oxygen gas when it is desired to impart hydrophilic properties to particles, fibers, etc. contained in the workpiece 5, and fluorine gas when it is desired to impart hydrophobic properties to particles, fibers, etc. contained in the workpiece 5.

[0062] <4> In the above embodiment, an example in which two ventilation holes 15c are provided has been described, but the number of ventilation holes 15c may be one, or may be three or more, and can be changed as appropriate. Furthermore, the positional relationship between the one or more ventilation holes 15c can also be changed as appropriate. For example, the one or more ventilation holes 15c may be provided closer to the end than to the center of the cover 1b.

[0063] <5> In the above embodiment, specific examples have been given of the revolution rotation speed and rotation speed of the agitation and degassing treatment device 100, the timing and duration of plasma irradiation to the workpiece 5, the plasma intensity, the shape of the nozzle 15a, etc., but these can be changed as appropriate.

[0064] <6> In the above embodiment, the control unit 4 continuously supplies the plasma-containing gas into the container 1 for at least a portion of the time during the rotation and revolution of the container 1. Alternatively, the control unit 4 may intermittently supply the plasma-containing gas from the plasma generation unit 2 into the container 1 for at least a portion of the time during the rotation and revolution of the container 1.

[0065] <7> In the above embodiment, the main body 1a of the container 1 is cylindrical with a bottom, but may have other shapes, such as a shape in which the diameters of the opening and the bottom are different. Also, in the above embodiment, a part of the plasma inducing unit 10 penetrates the center of the lid 1b and is inserted into the container 1. Alternatively, a part of the plasma inducing unit 10 may penetrate another part of the lid 1b.

[0066] <8> The configurations disclosed in the above embodiments (including other embodiments, the same applies below) can be applied in combination with configurations disclosed in other embodiments, as long as no contradictions arise. Furthermore, the embodiments disclosed in this specification are examples, and the embodiments of the present disclosure are not limited to these and can be modified as appropriate within the scope of the purpose of the present disclosure. [Industrial Applicability]

[0067] INDUSTRIAL APPLICABILITY The present disclosure can be used in an agitation / defoaming treatment device that is easy to use and has high agitation and defoaming performance, and in a production method for producing an agitated and / or defoamed object to be treated. [Explanation of symbols]

[0068] 1: Container 1a: Main body 1b: Lid body 1c: Ventilation hole 2: Plasma generating section 3: Gas supply source 4: Control section 5: Object to be treated 10: Plasma induction section 12: Rotating connector 13: Orbital section 14: Rotating connector 15: Rotation section 15a: Nozzle 15c: Ventilation hole 100: Mixing and defoaming equipment 106: Container holder D: Drive mechanism X1: Rotation axis X2: Revolution axis

Claims

1. An agitation and defoaming treatment apparatus including a container for accommodating a material to be treated therein, a container holder on which the container is mounted, and a drive mechanism for rotating the container holder about a rotation axis and revolving the rotation axis, a plasma guide unit that guides a plasma-containing gas into the container; The container includes a cylindrical main body having a bottom and an opening at an upper end, and a lid removably attached to the opening of the main body, a part of the plasma guide portion is inserted into the container through a central portion of the lid; The agitation and defoaming treatment device has an exhaust vent hole formed in the lid body at a position closer to the center portion than to the end portion of the lid body.

2. a plasma generating unit provided outside the container and configured to generate plasma; The agitation and defoaming treatment apparatus according to claim 1 , wherein the plasma guide section guides a gas containing plasma generated in the plasma generator section into the container.

3. the plasma guide unit includes a rotation unit attached to the container and rotatable in synchronization with the rotation of the container holder, a revolution unit rotatable in synchronization with the revolution of the container holder, and a rotary connector connecting the rotation unit and the revolution unit, 3. The agitation and defoaming treatment apparatus according to claim 2, wherein a gas containing plasma generated in the plasma generating section is introduced into the container via the revolving section, the rotary connector, and the rotating section.

4. 4. The agitation and defoaming treatment device according to claim 1, wherein the plasma induction unit has a nozzle inserted into the container and emitting a gas containing plasma.

5. The agitation and defoaming treatment device according to claim 4 , wherein the nozzle is disposed at a position where it does not come into contact with the object to be treated.

6. A production method for producing a processed object that has been stirred and / or degassed using a stirring and degassing treatment device including: a container that accommodates a processed object inside; a container holder on which the container is mounted; a drive mechanism that rotates the container holder about a rotation axis and revolves the rotation axis; and a plasma induction unit that introduces a plasma-containing gas into the container, The container includes a cylindrical main body having a bottom and an opening at an upper end, and a lid removably attached to the opening of the main body, a part of the plasma guide portion is inserted into the container through a central portion of the lid; The lid has an exhaust vent hole formed at a position closer to the center than to an end of the lid, The container that accommodates the object to be treated is rotated and revolved. The production method includes supplying the plasma-containing gas into the vessel for at least a portion of the time during the rotation and revolution.

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