KR100377237B1 - Plasma reactor and an apparatus containing the same - Google Patents

Abstract

The present invention relates to a plasma reactor and an apparatus including the same, and more particularly, to a reactor having an inlet of a carrier gas, a sample holder to which a sample can be attached, a venting valve, and a cover simplified by concentrating a pump and gauge connection unit. The particulate sample relates to a plasma reactor in which a magnetic bar is inserted into the reactor to allow the magnetic bar to rotate together with the particulate sample. The reactor according to the present invention can efficiently process various types of samples, respectively or simultaneously, and enables uniform surface treatment.

Description

Plasma reactor and an apparatus containing the same

The present invention relates to a plasma reactor and a device including the same, and more particularly, a plasma having an inlet of a carrier gas, a sample holder for attaching a sample, a venting valve, and a cover simplified by concentrating a pump and gauge connection unit. In the case of the reactor and the particulate sample relates to a plasma reactor in which a magnetic bar is inserted into the reactor so that the magnetic bar can be rotated together with the particulate sample.

Recently, researches to maximize the properties of polymers by modifying the surface of polymer materials are actively underway. The modified polymer may be used in various fields by modifying the surface of the polymer material to not only have the properties of the original polymer but also add other functional functional groups. There are many ways to modify the surface of the polymer, but recent research has been focused on easily modifying the surface using plasma. The use of plasma has the advantage of being cost effective and having a certain treatment effect since no additional process is introduced compared to other surface modification methods.

However, in the existing studies, the shape of the polymer sample is mainly limited to the shape of the film or the fibrous form (Boening, H. V., Fundamentals of plasma chemistry and tech Technomic Pub., Lancaster (1988)). However, since the polymer in the form of film or fiber is fixed to a specific part in the reactor, only the part in contact with the plasma is modified so that the surface is not uniformly treated.

Until now, studies on the surface modification of polymer particles have been insignificant, and conventional methods for surface treatment have been made of fixed layers having difficulty in intimate contact of the particles with plasma. Thus, recently, a fluidized reactor capable of improving the mixing characteristics of polymer particles and plasma and capable of treating all surfaces of particles has been studied. Anand, M., RE Cohen and RF Baddour, "Surface modification of low density polyethylene in a fluorine gas plasma", Anand et al (1981), polymer , 22, 361-371 (1981); US Patent No. 4,264,750 (1981) describes a vibrating fluidized bed reactor for modifying polyethylene particles in CF ₄ plasma, but the melting point of the plasma treated particles does not change, but the surface properties are deformed. .

In addition, Kusakabe et al (1989), Kusakabe, K., T. Kuriyama and S. Morooka, "Fluidization of fine particles at reduced pressure", Powder Technol ., 58, 125-130 (1988), described in SiC, TiO. ₂ , It is described that the fine particles of Ni naturally form agglomerates in a reduced pressure fluidized bed, and these are particles of Geldart's group A.

Based on the results, Okubo et al (1990) by Okubo, T., H. Kawamura, K. Kusakabe and S. Morooka, "Plasma nitriding of titanium particles in afluidized bed reactor at a reduced pressure", J. Am . Ceram. Soc ., 73, 1150-1152 (1990) describe a method of nitriding titanium particles in a reactor using a nitrogen plasma and applying rf power of 13.56 MHz to the reactor. When titanium particles of 46 to 74 mu m are flowed at 923 K, the nitriding rate is increased by 2-3 times by the plasma.

U.S. Pat. No. 4,810,524 to TDK Co. also describes a process for forming thin films by plasma polymerization of inorganic particles, in particular magnetic powder. This process takes the form of plasma being sprayed towards the particles while the reactor is rotating.

Japanese Patent Laid-Open No. 5-7177342 (1983) by Toshiba Co. introduces a device for plasma treatment of particles, including a microwave generator, a microwave transmission antenna, and a gas supply for electric discharge. A device, a rotating cylinder, and a vacuum pump can be mentioned. Masuoka, T., O. Hirasa and Y. Suda, "Plasma surface treatment apparatus for powdery materials" by Masuoka et al (1984), Bull. Res. Inst. Polym. Text. (Jpn) , 144, 73-77 (1984), describes a method using a rotary kiln as a plasma reactor to coat particles with a polymer film.

Representative plasma reactors of the prior art described above are shown in FIGS. FIG. 6 is a fluidized bed plasma reactor, which is a reactor that fills particles in a reactor and injects gas under the reactor to float the particles. Since the plasma is generated in the region in which the particles flow, there is an advantage of good contact between the polymer particles and the plasma. However, if the particle size is large, there is a disadvantage that a large amount of gas is required to flow the particle, and larger particles have a problem that cannot flow. In addition, FIG. 7 is a kiln-type reactor in which the reactor is rotated to make good contact between the polymer particles and the plasma. This is a complicated apparatus compared to other reactors because of the direct rotation of the reactor, which makes it difficult to maintain a vacuum in the reactor. 8 shows a fixed bed reactor, in which a sample in a film form is fixed to a stator and the surface is modified by moving the sample to a plasma generating position, but the reactor is fixed so that the reaction between the plasma and the sample is compared with that of the other. However, there is a disadvantage in that the surface is modified only in the portion exposed to the plasma.

Although the reactors described above are the most widely used plasma reactors to date to those skilled in the art, they have the disadvantage that only one type of sample can be processed. That is, the fluidized bed reactor and the kiln type reactor can process only a particulate sample, and the fixed bed reactor is a reactor capable of processing only a sample in the form of a film.

Accordingly, the present inventors solved the problems of the above-described reactors, and as a result of studying a reactor capable of processing various types of samples, respectively or simultaneously, the present inventors completed the plasma reactor of the present invention.

Accordingly, an object of the present invention is to solve the problems of the above-described reactors and to provide a plasma reactor having a simplified reactor structure capable of processing various or different types of samples, respectively, and a device including the same.

Plasma reactor of the present invention for achieving the above object is a reactor and particulate sample having a simplified cover by integrating a carrier gas inlet, a sample holder to which the sample can be attached, a venting valve, and the pump and gauge connections A magnetic bar is placed inside the reactor to allow the magnetic bar to rotate with the particulate sample.

1 is a schematic diagram of a plasma reactor according to the present invention,

2 shows a sample holder used in the plasma reactor according to the present invention,

3a to 3c show a plan view, a side cross-sectional view and a bottom view, respectively, of a reactor lid according to the invention,

4 is a schematic view showing a state of processing a sample in the form of a film in an example plasma reactor according to the present invention,

5 is a schematic view showing a state of processing a polymer sample in the form of particles in an example plasma reactor according to the present invention;

6 to 8 show a conventional plasma reactor.

Explanation of the main symbols in the drawings

1: sample holder 2: gas inlet

3: pump and gauge connection 4: reactor cover

5: magnetic bar 6: magnetic stirrer

7: plasma reactor 8: O-ring

9: cooling fan 10: venting valve

11: sus edition

Hereinafter, the present invention will be described in more detail with reference to the accompanying drawings, but the scope of the present invention is not limited thereto.

Figure 1 is a schematic diagram of a plasma reactor according to the present invention, the apparatus of the present invention can be divided into five parts into a reactor portion, a carrier gas inlet portion, a vacuum system portion, a plasma matching system and a magnetic stirrer.

The reactor section is made of Pyrex glass tubes, and the bottom of the reactor is designed to be elliptical for more efficient flow of polymer particles such as HDPE.

In the matching network, since the particles are not fixed in the reactor but flow, the auto matching network is used in consideration of the effect of the plasma state and the rotational speed of the magnetic bar. In addition, the vacuum system uses a rotary pump (RP) and a diffusion pump (DP) to maintain a high vacuum. The magnetic bar is rotated in the reactor by flowing a magnetic field using a magnetic stirrer to flow the particles. As a carrier gas, argon, oxygen, hydrogen, fluorine, or the like may be used.

In the experimental method using the plasma reactor according to the present invention as shown in FIG. 1, a magnetic bar 5 and a particulate polymer sample are placed in the reactor 7, and a vacuum pump is used to vacuum the pressure in the reactor. After the vacuum, the vacuum for about 10 minutes to reduce the reactor pressure to less than 10mTorr, the carrier gas is injected into the reactor to maintain the desired pressure to proceed with the reaction and using a magnetic stirrer to rotate the polymer particles together with the magnetic bar. When the pressure in the reactor is kept constant, the plasma is turned on to react for the desired time. After the reaction is completed, the plasma is turned off and gas is flowed in the reactor for about 10 minutes. This is to prevent other impurities from adsorbing to the long-lived radicals remaining on the sample surface after the reaction. Finally, the gas is exhausted through the vent valve 10 to bring the pressure to atmospheric pressure before taking the sample out. In the case of treating the sample in the form of a film using the sample holder 1, the experiment is performed in the same manner as in the above method except that the magnetic bar 5 is not used and the magnetic stirrer is not operated. In addition, when simultaneously processing a particle and a sample in the form of a film, the sample holder 1 and the magnetic bar 5 are used together.

Figure 2 shows a state in which a sample in the form of a film fixed to the sample holder 1 used in the plasma reactor of the present invention. The sample in the form of a film may be attached to a sample holder, and then placed in a reactor to react with the plasma, and the reaction position with the plasma may be adjusted by moving the holder up and down.

3a to 3c show a reactor cover 4 according to the invention, in which FIG. 3a shows a plan view, FIG. 3b shows a side sectional view and FIG. 3c shows a bottom view. In the present invention, the vacuum is maintained by using an O-ring (8) for the vacuum between the reactor and the cover, and the sample holder (1) is fixed at the center and the pump and gauge connection (3), gas Inlet (2), venting valve 10 is located. As such, the device of the present invention is easy to handle the sample by attaching the cover 4 to the reactor made of Pyrex, as well as the inlet of the gas, sample holder, venting valve and pump and gauge connection to the reactor cover is concentrated. Device is simplified. In addition, the sample in the form of a film can be attached to the sample holder for processing, the position of the sample in the plasma can be changed by moving the sample holder up and down, the magnetic bar is put into the reactor for the sample in the form of a particle, the reactor itself The particles can be flowed by the rotation of the magnetic bar without rotating. As such, since the reactor does not rotate, the apparatus is simple, and there is an advantage that the size of the particles is not limited as in the fluidized bed reactor.

Figure 4 is a schematic diagram showing a state of processing a sample in the form of film in an example plasma reactor according to the present invention, as shown in order to wind the coil around the reactor to generate a plasma, to lower the heat generated during the reaction The cooling fan 9 can also be attached. In addition, in order to prevent the plasma magnetic field generated in the reactor from being transmitted to the outside, the outside of the reactor is blocked by a sus plate 11 made of stainless steel.

In addition, Figure 5 is a schematic diagram showing a state of processing the polymer sample in the form of particles in an example plasma reactor according to the present invention, by flowing a magnetic polymer particles in the magnetic stirrer by rotating the magnetic bar.

The types of polymer samples that can be processed according to each reactor type can be briefly summarized in Table 1 below.

Fluidized bed reactor Kiln reactor Fixed bed reactor Reactor according to the invention powder ○ ○ × ○ film × × ○ ○ Particles × ○ × ○

As described above, the reactor according to the present invention has a carrier gas inlet, a sample holder, a pump and gauge connection portion, and a venting valve are integrated in the cover of the reactor, thereby simplifying the apparatus, and in a variety of film, powder or particle forms. The polymer sample in the form can be processed individually or simultaneously, and there is no need to rotate the reactor, so the device is simple and has the advantage of not being limited by the size of the particles as in a fluidized bed reactor.

Claims (8)

A plasma reactor comprising a reactor having an inlet of a carrier gas, a sample holder to which a sample can be attached, a venting valve and a cover simplified by concentrating a pump and a gauge connection, and a magnetic bar located inside the reactor. A plasma reactor, comprising: an inlet for a carrier gas, a sample holder for attaching a sample in the form of a film, a venting valve, and a cover simplified by concentrating a pump and gauge connection. The plasma reactor according to claim 1 or 2, wherein the bottom surface of the reactor is elliptical. The plasma reactor according to claim 1 or 2, wherein the reactor is made of Pyrex. The plasma reactor according to claim 1 or 2, wherein a cooling fan can be further attached to the outside of the reactor. The plasma reactor according to claim 1 or 2, further comprising a sustain plate made of stainless material outside the reactor. The plasma reactor of claim 1 and a carrier gas inlet device for introducing carrier gas into the reactor, a vacuum system including a pump for maintaining the vacuum of the reactor below 10 mTorr, the plasma state according to the flow of particles and the rotational speed of the magnetic bar Plasma reactor comprising a matching system to adjust and a magnetic stirrer for particle flow. The plasma reactor of claim 2 and a carrier gas inlet device for introducing a carrier gas into the reactor, a vacuum system including a pump for maintaining the vacuum degree of the reactor below 10 mTorr, the plasma state according to the flow of particles and the rotational speed of the magnetic bar Plasma reactor comprising a matching system to adjust and a magnetic stirrer for particle flow.