KR101613432B1 - A equipment of modifying a surface in a polymer tube inner side and a surface modifying method therewith - Google Patents

A equipment of modifying a surface in a polymer tube inner side and a surface modifying method therewith Download PDF

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KR101613432B1
KR101613432B1 KR1020140126962A KR20140126962A KR101613432B1 KR 101613432 B1 KR101613432 B1 KR 101613432B1 KR 1020140126962 A KR1020140126962 A KR 1020140126962A KR 20140126962 A KR20140126962 A KR 20140126962A KR 101613432 B1 KR101613432 B1 KR 101613432B1
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South Korea
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polymer tube
electrode
reaction gas
unit
polymer
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KR1020140126962A
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Korean (ko)
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KR20160035682A (en
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조용기
문경일
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한국생산기술연구원
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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Treatments Of Macromolecular Shaped Articles (AREA)
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Abstract

The present invention relates to a surface modification apparatus and a surface modification method of a polymer tube inner surface, which comprises forming a reactive active species that makes hydrophilic or lipophilic (hydrophobic) inner surface of a small-diameter polymer tube by combining vacuum and plasma discharge technology A vacuum forming unit for vacuuming the inner surface of the polymer tube and the polymer tube, a reaction gas supply unit for supplying the reaction gas for forming the reactive active species to the inner surface of the polymer tube, and an electrode And a transfer unit having a function of moving the polymer tube relative to the polymer tube in the longitudinal direction, wherein the inner surface of the polymer tube is a closed space in the process of the inner surface treatment of the polymer tube, A surface modification apparatus for the inner surface of a polymer tube and a surface modification method using the same The deadline.

Description

Technical Field [0001] The present invention relates to an apparatus for modifying a surface of a polymer tube and a method for modifying a surface using the same.

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a surface modifying apparatus and a surface modifying method for improving the quality of an inner surface of a polymer tube, and more particularly, to a surface modifying apparatus and a surface modifying method, The present invention relates to a surface modification apparatus and a surface modification method for an inner surface of a polymer tube, and more particularly, to a surface treatment using a dielectric barrier discharge (DBD).

The surface treatment of a polymer tube used in conventional medical applications is performed by a method of etching a polymer surface with a chemical substance and then depositing a drug, which is referred to as a wet process for surface modification. In recent years, low temperature plasma technology has been used for surface treatment of tubes that modify the outer surface of a large diameter tube or have a small aspect ratio pattern on the surface. The reactive active species formed by plasma discharge of the reactive gas are formed on the surface of the polymer material to improve the material properties-hydrophobicity, hydrophilicity, dyeability, adhesion and the like. Many applications are being made.

In Korean Patent No. 0449524 (entitled " Plasma Processing Method and Apparatus ", hereinafter referred to as Prior Art 1), in plasma processing, a dielectric tube attached to a metal body fixed to a vacuum container The vacuum vessel is evacuated from the vacuum vessel while introducing gas into the vacuum vessel through the hole of the vacuum vessel and the high frequency power having a frequency in the range of 100 kHz to 3 GHz is supplied to the substrate mounted on the substrate electrode in the vacuum vessel A plasma is generated in a vacuum chamber by applying the plasma to a plasma source which is installed so as to face the substrate.

KR 0449524 B

In the prior art 1, a gas is introduced into a vacuum vessel through a hole of a dielectric tube attached to a metal body fixed to the vacuum vessel, and exhausted from the vacuum vessel, and the dielectric tube protruded by 0.5 to 20 mm from the surface of the metal body Maintaining the vacuum vessel within a predetermined pressure; And a step of applying a high frequency power having a frequency in the range of 100 kHz to 3 GHz to a plasma source arranged so as to face a substrate mounted on a substrate electrode in a vacuum container to generate plasma in the vacuum container to perform plasma treatment of the substrate However, there is a disadvantage that a high voltage is required for discharging, and there is a problem that ozone is generated during the reaction. Further, there is a problem that it is difficult to apply to the inner surface of a small-diameter tube.

In a polymer tube inner surface treatment apparatus,

A polymer tube and a vacuum forming part for forming an inner surface of the polymer tube in a vacuum state, a reaction gas supplying part for supplying a reaction gas for forming a reactive active species to the inner surface of the polymer tube, and an electrode part having a function of plasma- And a transfer part having a function of moving the polymer tube in the longitudinal direction, wherein the inner surface of the polymer tube becomes an airtight space during the inner surface treatment process of the polymer tube, The surface modification apparatus of the present invention.

Further, in the surface treatment method using the surface modifying apparatus on the inner surface of the polymer tube,

A step S30 of placing a polymer tube in a transfer part, a step S20 of evacuating the inner surface of the polymer tube, a step S30 of forming a predetermined pressure on the inner surface of the polymer tube by injecting a predetermined reaction gas into the polymer tube, and A step S40 of generating a plasma only around the electrode by applying a dielectric barrier discharge (DBD) to the electrode part, and a step S50 of continuously moving the polymer tube in the longitudinal direction by moving the polymer tube by driving the transfer part, ;

The present invention also provides a method for modifying the surface of an inner surface of a polymer tube.

Also provided is a polymer tube whose inner surface has been modified using the surface modification method of the present invention.

The present invention relates to a surface modifying apparatus and a surface modifying method for improving the characteristics of the inner surface of a polymer tube, and more particularly, to a surface modifying apparatus and a surface modifying method for improving surface characteristics of a polymer tube by surface- And the device. Accordingly, the inner surface of the polymer tube is modified to be hydrophilic or lipophilic, and thus the polymer can be used in medical polymer tubes capable of drug impregnation. Also, plasma is induced only in the vicinity of the electrode due to the dielectric barrier discharge (DBD), thereby improving the surface characteristics of the inner surface of the polymer container.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic view showing a surface modifying apparatus for treating the inner surface of a polymer tube of the present invention. FIG.
2 is a schematic view of an adapter connecting the polymer tube of the present invention to a vacuum forming part or a reaction gas supplying part.
3 is a schematic diagram of plasma generation on the inner surface of the tube of the present invention.
4 is a schematic view and a schematic view showing a plasma discharge using the dielectric electrode of the present invention.
FIG. 5 is an explanatory view in which the inner surface of the polymer tube of the present invention changes from a hydrophilic material to a hydrophilic material after the reaction.

Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings.

The polymer tube 100 is preferably made of a flexible dielectric. This flexibility makes it possible to use devices such as winding rolls in the manufacturing process. In addition, when the electric field 510 is formed in the polymer tube as a dielectric, a displacement field is formed inside the polymer tube. Using this characteristic, a plasma surface discharge as described later is induced. The material of the polymer tube 100 may be any one selected from PTFE, FEP, PFA, PE, Silicone, PDMS, PU, and ethylene vinyl acetate (EVA), or a copolymer thereof.

The vacuum forming unit 200 is required to have a function of evacuating the inner surface of the polymer tube 100. In an embodiment shown in FIG. 1, a first valve 210 is provided in the vacuum forming unit In the state where the first valve 210 is open, the pump is operated to vacuum the inner surface of the polymer tube, and then the first valve is closed to maintain the vacuum state. Further, one end of the conduit is extended from the first valve and connected to the polymer tube. At this time, an adapter to be described later is required for sealing connection between the conduit and the polymer tube.

The reaction gas supply unit 300 functions to supply a reaction gas into the polymer tube. The reaction gas may be any one selected from Ar, H 2 , C 2 H 2 , N 2 , O 2, and He, But it is not limited to this, and various other inert gases and active gases may be supplied. The kind of the reaction gas to be added should be determined according to the material of the polymer tube and the type of the reactive active species to be produced. 1, the reaction gas supply unit includes a mass flow controller (MFC) 330 and a second valve (gas supply valve 1) 310 for controlling the supply of each of the individual reaction gases. And a third valve (gas supply valve 2) 320 for controlling whether or not the reaction gas is finally input and supplied. The reaction gas, which is controlled by these elements and is introduced into the polymer tube 100, finally forms a predetermined partial pressure (generally, a pressure lower than atmospheric pressure) in the polymer tube. Further, one end of the conduit must extend from the third valve to be connected to the polymer tube. At this time, an adapter to be described later is required for sealing connection between the conduit and the polymer tube.

The electrode unit 400 functions to form a reactive active species by causing a plasma discharge to the reaction gas. The electrode unit may include a first electrode (input electrode) 410 and a second electrode (dielectric electrode) 420, and may further include a third electrode (ground electrode) 430. In particular, due to the presence of the second electrode made of a dielectric material, a dielectric barrier discharge (DBD) is triggered to generate a surface discharge around the electrode, and the second electrode (dielectric electrode) 420 The material may be ceramic or polymeric.

In a normal atmospheric pressure discharge (corona discharge), a current is induced with respect to an applied voltage of AC, and the induced current is mainly distributed in a range of -100 mA to 100 mA. On the contrary, according to the structure of the present invention, the displacement field is formed in the interior of the high dielectric constant (dielectric constant r> 5) by the electric field formed by the power source part 500, On the inner surface of the tube, a surface discharge is induced by the displacement field of the inherent whole.

The power unit is connected to the electrode unit 400 and performs a function of applying a voltage to the electrode unit. The voltage at this time is AC, and this AC voltage acts to induce a current of another sign by the surface discharge on the inner surface of the polymer tube 100. 4, when the electric field 510 is applied, a displacement field is formed in the dielectric, and a plasma discharge is induced by being charged by this displacement field. The reaction gas filled in the polymer tube in the vacuum state is vibrated by the applied displacement field and is excited and ionized. A surface discharge current having an opposite sign to the applied current is formed from the surface discharge induced by the magnetic field change. In addition, dissociated ions and electrons are trapped and released into the electrode. At this time, the asymmetric structure (phase difference) of voltage and current due to the self bias generated due to the difference in the mass ratio between the collected particles and the discharged particles appear.

In the present invention, in the surface treatment of the polymer tube, it is necessary that the inside of the polymer tube becomes a closed space, in order to prevent inflow of gas other than the reaction gas introduced under vacuum. In order to ensure this, an adapter is required which is installed between the polymer tube and the vacuum forming part, and between the polymer tube and the reaction gas supplying part, and performs the function of connecting these elements. In other words, the diameter (diameter) of one end of the polymer tube 100 is different from the diameter (diameter) of the conduit extending from the vacuum forming part 200 / reaction gas supplying part 300, Since it is difficult to join them, an adapter 700 is required as a mechanical device for connecting the two. The adapter should have an insertion portion of a conduit extending from the vacuum forming portion / reaction gas supplying portion and an insertion portion capable of inserting one end of the polymer tube as shown in the schematic diagram of FIG. 2. After the insertion, the adapter / The clearance of the adapter should be removed. Such an adapter only functions to connect the polymer tube and the vacuum forming unit / reaction gas supplying unit, and connection / disconnection with the vacuum forming unit / reaction gas supplying unit is performed through separate valve elements 210 and 320 .

The transfer section performs a function of moving the polymer tube and the electrode section relative to each other in the longitudinal direction of the polymer tube. The size of the second electrode may be set to an appropriate size to reduce the plasma surface discharge region, and the polymer tube or the electrode portion may be relatively , It is advantageous in view of cost, process efficiency and productivity. The configuration of the transfer section may be a system (tube transfer system) in which the electrode unit is fixed and the polymer tube is transferred, or a system in which the polymer tube is fixed and the electrode unit is transferred (electrode unit transfer system) may be adopted.

In the embodiment shown in FIG. 1, in order to improve the productivity when the tube transferring system is adopted, the transfer part includes a first winch (unlocking winch) 610 connecting the one end of the polymer tube 100, a polymer tube And a second winch (winding winch 620) and an auxiliary roller 650 for connecting the other end of the first winch 100 to the second winch. However, it does not exclude the method of transporting the prepared polymer tube in a flat manner on a flat surface in a pulling manner.

In addition, such a transfer unit may be configured to perform the function of the above-described adapter at the same time. 1, a first winch (unlocking winch) 610 is formed by allowing a polymer tube to be wound around the outer periphery thereof, forming a cavity therein, And a polymer tube is inserted into the cavity so that the reaction gas supply part and the polymer tube are connected to each other through the cavity. The second winch (winding winch) 620 is configured to allow the polymer tube to be wound around the outer periphery thereof, to form a cavity therein, and then to insert a conduit extending from the vacuum forming portion 300 toward the cavity And the polymer tube is inserted toward the cavity, and as a result, the vacuum forming part and the polymer tube are connected to each other via the cavity. Of course, it is also possible to connect the vacuum forming part to the first winch side. As a result, the first winch and the second winch will eventually also function as so-called first adapter 710 and second adapter 720.

The surface modifying apparatus for the inner surface of the polymer tube may further include a measuring unit 800 for measuring and displaying the degree of vacuum or the partial pressure of the reaction gas inside the polymer tube. The information on the degree of vacuum / the partial pressure of the reactive gas may be displayed on the measuring unit 800 by the driver or may be transmitted to the automatic controller, The feedback control for generating the drive signal of the valve / actuator may be possible.

Hereinafter, a method for modifying the inner surface of the polymer tube 100 will be described.

First, the polymer tube 100 is placed in the transfer unit 600. In this step, the inside of the polymer tube can be formed as a closed space. Second, the inner surface of the polymer tube 100 is evacuated. Third, a predetermined reaction gas is introduced until a predetermined partial pressure is formed inside the polymer tube. Fourth, a voltage is applied to the electrode portion to generate a dielectric barrier discharge (DBD) plasma. That is, when the electric field 510 is applied to the second electrode (dielectric electrode) by the AC voltage, the magnetic field 440 is induced and the reactive gas is discharged on the plasma surface to form a reactive active species, which is adsorbed on the inner surface of the high- Surface modification is performed. Fifthly, a step of continuously treating the inner surface of the polymer tube with respect to the longitudinal direction while driving the transfer part to move the polymer tube relative to the electrode part. In the embodiment, this is accomplished by winding using a winch.

3, a predetermined voltage is applied to the polymer tube 100 in order to generate a plasma. In the surface modification method of the inner surface of the polymer tube 100, And the inner surface is vacuumed by the forming portion 200. Thereafter, when an AC voltage is applied in the power source unit 500 according to time, a displacement field is induced in the high dielectric constant electrode unit 420, and the displacement field induces a surface discharge inside the polymer tube 100. The polymer tube 100 has a negative value with respect to the applied current at the time of surface discharge and no discharge is generated at the outer surface of the polymer tube 100. It is preferable that a reactive active species (for example, Surface treatment, hydrocarbons or carbon oxide deposition, etc.) can be formed.

Surface treatment with reactive reactive species is accomplished through deposition of hydrocarbons and carbon oxides. These reactive active species are modified to hydrophilic or lipophilic on the inner surface of the polymer tube 100. 5, Ar / C2H2 was injected as a reactive gas into a PTFE polymer tube (inner diameter: 2.3 mm) having a hydrophobic surface to induce a plasma surface discharge, thereby forming a hydrocarbon thin film And was modified to be hydrophilic. Further, in the second embodiment, the Ar was supplied for 10 seconds C2H2 and inert gas of Ar to the PE polymer tube having a hydrophobic surface, and further supplied 10 seconds Finally, O 2 for 10 seconds supplied by reforming the tube surface to a hydrophilic Respectively.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it should be understood that various changes and modifications will be apparent to those skilled in the art. Obviously, the invention is not limited to the embodiments described above. Therefore, the scope of protection of the present invention should be construed in accordance with the following claims, and all technical ideas which fall within the scope of the invention by changing, substituting, substituting, etc. without departing from the gist of the present invention, It is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents. Also, it should be clarified that some of the drawings are intended to illustrate the structure more clearly and are provided in an exaggerated or reduced size than the actual one.

100. Polymer tube
200. Vacuum forming part
210. First valve (vacuum valve)

300. Reaction gas supply part
310. Second valve (gas supply valve 1)
320. Third valve (gas supply valve 2)
330. Gas flow control device (MFC)


400. Electrode portion
410. First electrode (metal electrode)
420. Second electrode (dielectric electrode)
430. Third electrode (ground electrode)
440. Magnetic field


500. Power supply
510. Electric field


600. Transfer Section
610. 1st winch (winch winch)
620. 2nd winch (winding winch)
650. Auxiliary roller


700. Adapter
710. First adapter
720. Second adapter


800. Measuring section

Claims (14)

A surface treatment apparatus for a polymer tube,
A polymer tube (100);
A vacuum forming part 200 for forming a vacuum state in the polymer tube 100;
A reaction gas supply unit 300 for supplying a reaction gas for formation of a reactive active species;
An electrode unit 400 having a function of discharging the reaction gas to plasma;
A power supply unit 500 for applying a voltage to the electrode unit 400; And
A transfer unit 600 having a function of relatively moving the polymer tube 100 and the electrode unit 400 in the longitudinal direction;
, ≪ / RTI >
Wherein the inside of the polymer tube is a closed space in a surface treatment process of the polymer tube (100). The method according to claim 1,
The surface modification apparatus for the inner surface of the polymer tube is installed between the polymer tube 100 and the vacuum forming unit 200 and between the polymer tube 100 and the reaction gas supply unit 300, 100) having a function of forming a closed space in the inside of the polymer tube. The method according to claim 1,
The transfer unit 600 includes a first winch (winding winch) connected to one end of the polymer tube 100 and a second winch (unlocking winch) connected to the other end of the polymer tube 100 And the surface of the inner surface of the polymer tube is modified. The method of claim 3,
The transfer unit 600 is installed between the polymer tube 100 and the vacuum forming unit 200 and between the polymer tube 100 and the reaction gas supply unit 300, Of the inner surface of the polymer tube. The method according to claim 1,
The apparatus for surface modification of an inner surface of a polymer tube according to claim 1, further comprising a measuring unit (800) for measuring and displaying a degree of vacuum or a partial pressure of a reaction gas inside the polymer tube (100). The method according to claim 1,
Wherein the polymer tube (100) is made of a flexible dielectric material. The method of claim 6,
Wherein the polymer tube 100 is made of one of PTFE, FEP, PFA, PE, PDMS, PU, Silicone, and ethylene vinyl acetate (EVA) or a copolymer thereof. The method according to claim 1,
The electrode unit (400) includes a first electrode (metal electrode) and a second electrode (dielectric electrode). The method of claim 8,
Wherein the material of the second electrode (dielectric electrode) is a ceramic-based or polymer-based material. The method according to claim 1,
Wherein the reaction gas supplied from the reaction gas supply unit 300 is any one selected from the group consisting of Ar, H 2 , C 2 H 2 , N 2 , O 2, and He, or a mixed gas thereof. Surface modifying device. The method according to claim 1,
Wherein the reaction gas supply unit (300) comprises a gas flow rate controller (MFC). A surface treatment method using a surface modifying apparatus for an inner surface of a polymer tube according to any one of claims 1 to 11,
(S10) placing the polymer tube 100 in the transfer part 600;
(b) evacuating the inside of the polymer tube 100 by vacuum (S20);
(c) injecting a predetermined reaction gas into the polymer tube 100 until a predetermined partial pressure is formed in the polymer tube 100 (S30);
(d) applying a voltage to the electrode unit 400 to generate a dielectric barrier discharge (DBD) plasma (S40); and
(S50) of continuously treating the inner surface of the polymer tube with respect to the longitudinal direction while moving the polymer tube (100) relative to the electrode unit (400) by driving the transfer unit (600);
Wherein the inner surface of the polymer tube is made of a thermoplastic resin. The method of claim 12,
Wherein the inner surface of the polymer tube (100) is modified to be hydrophilic or lipophilic by the reaction gas. A polymer tube (100) having an inner surface modified by using the surface modification method of claim 12.
KR1020140126962A 2014-09-23 2014-09-23 A equipment of modifying a surface in a polymer tube inner side and a surface modifying method therewith KR101613432B1 (en)

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KR1020140126962A KR101613432B1 (en) 2014-09-23 2014-09-23 A equipment of modifying a surface in a polymer tube inner side and a surface modifying method therewith

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100217538B1 (en) 1996-04-10 1999-09-01 박호군 Method for modifying a surface of polymeric material using plasma source ion implantation and apparatus therefor
KR100443655B1 (en) 2001-05-28 2004-08-09 장성근 Surface treatment method of polymer resin-based molded products by using low temperature and atmospheric pressure plasma
KR100449524B1 (en) 2000-08-04 2004-09-21 마츠시타 덴끼 산교 가부시키가이샤 Plasma processing method and apparatus thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100217538B1 (en) 1996-04-10 1999-09-01 박호군 Method for modifying a surface of polymeric material using plasma source ion implantation and apparatus therefor
KR100449524B1 (en) 2000-08-04 2004-09-21 마츠시타 덴끼 산교 가부시키가이샤 Plasma processing method and apparatus thereof
KR100443655B1 (en) 2001-05-28 2004-08-09 장성근 Surface treatment method of polymer resin-based molded products by using low temperature and atmospheric pressure plasma

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