KR20010019025A - An apparatus for forming polymer continuously on the surface of metal by dc plasma polymerization - Google Patents

An apparatus for forming polymer continuously on the surface of metal by dc plasma polymerization Download PDF

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Publication number
KR20010019025A
KR20010019025A KR1019990035224A KR19990035224A KR20010019025A KR 20010019025 A KR20010019025 A KR 20010019025A KR 1019990035224 A KR1019990035224 A KR 1019990035224A KR 19990035224 A KR19990035224 A KR 19990035224A KR 20010019025 A KR20010019025 A KR 20010019025A
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South Korea
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sample
chamber
unwinding
plasma polymerization
voltage
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KR1019990035224A
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Korean (ko)
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정영만
이수원
김철환
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구자홍
엘지전자 주식회사
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Priority to KR1019990035224A priority Critical patent/KR20010019025A/en
Publication of KR20010019025A publication Critical patent/KR20010019025A/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/62—Plasma-deposition of organic layers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32018—Glow discharge
    • H01J37/32027—DC powered
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32431—Constructional details of the reactor
    • H01J37/32733—Means for moving the material to be treated
    • H01J37/32752—Means for moving the material to be treated for moving the material across the discharge
    • H01J37/32761—Continuous moving
    • H01J37/3277—Continuous moving of continuous material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32917—Plasma diagnostics
    • H01J37/3299—Feedback systems
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/32—Processing objects by plasma generation
    • H01J2237/33—Processing objects by plasma generation characterised by the type of processing
    • H01J2237/338—Changing chemical properties of treated surfaces
    • H01J2237/3382—Polymerising

Abstract

PURPOSE: A continuous plasma polymerization device is provided to form uniformed polymerization films on both sides of a sample, thereby forming a reliable polymerization film by introducing to an existing continuous plasma polymerization device a voltage controller as a means which maintains voltages between each electrode oppositely directed to both sides of samples equal. CONSTITUTION: A continuous plasma polymerization device comprises an unwinding chamber (21) including an unwinding roll (20) unwinding a sample (2) of which surface is treated in order to transfer to other chamber, a deposition chamber (1) in which separate electrodes oppositely directed to upper and lower sides of the sample (2) introduced from an unwinding roll (20) of the unwinding chamber (21) are installed, a voltage controller for maintaining each voltage between each electrode oppositely directed to the sample (2) and the sample (2) equal is introduced, and both sides of the sample (2) are polymerized by plasma, a winding chamber (23) including a winding roll (22) winding the sample (2) of which surface is treated in the deposition chamber (1), a pumping means for maintaining the deposition chamber (1) in vacuum, and a gas inlet introducing a reactive gas and a non reactive gas.

Description

플라즈마중합 연속처리장치{AN APPARATUS FOR FORMING POLYMER CONTINUOUSLY ON THE SURFACE OF METAL BY DC PLASMA POLYMERIZATION}Plasma polymerization continuous processing equipment {AN APPARATUS FOR FORMING POLYMER CONTINUOUSLY ON THE SURFACE OF METAL BY DC PLASMA POLYMERIZATION}

본 발명은 플라즈마중합 연속처리장치에 관한 것이다.The present invention relates to a plasma polymerization continuous processing apparatus.

플라즈마를 이용하여 금속판 등의 시료 표면을 박막코팅 처리하면 경도, 내마모성 등이 뛰어난 피복층이 형성된다. 피복층이 형성된 제품은 자기디스크, 광디스크, 초경질공구 등으로 사용된다. 또한 강철판 표면에 형성된 도장막에 플라즈마처리를 하면 경질화되고, 내구성, 내식성 등이 뛰어난 도장 강판이 얻어진다. 특히, 시료 표면에 고분자중합처리를 하여 친수성 또는 소수성을 향상시키는 표면개질 효과를 얻을 수 있으며, 이렇게 표면개질된 물질은 다양한 범위에 응용되고 있다.When a thin film is coated on the surface of a sample such as a metal plate using plasma, a coating layer having excellent hardness, wear resistance, and the like is formed. Products with a coating layer are used for magnetic disks, optical disks, ultra hard tools, and the like. In addition, when the coating film formed on the surface of the steel sheet is subjected to plasma treatment, the coated steel sheet is hardened and excellent in durability, corrosion resistance and the like is obtained. In particular, the surface modification effect of improving the hydrophilicity or hydrophobicity can be obtained by polymerizing the surface of the sample, and the surface-modified material has been applied to various ranges.

플라즈마중합장치의 대표적인 예로는 WO99/28530에 개시된 장치가 있다.(도 1 참조) 상기 장치의 구성은 크게 진공 챔버(1), 챔버 내에 설치된 전극(4), 진공 챔버의 압력을 조절하기 위한 진공 펌프(5, 6), 진공도를 측정하기 위한 계기(7, 8), 전극에 전위차를 발생시키기 위한 전력공급장치(3), 표면처리 하고자 하는 시료 주위에 반응성 가스 및 질소와 같은 비반응성 가스를 주입하는 반응 가스 조절장치(9, 10) 등으로 이루어져 있다.A typical example of the plasma polymerization apparatus is the apparatus disclosed in WO 99/28530. (See FIG. 1) The configuration of the apparatus is largely a vacuum chamber 1, an electrode 4 installed in the chamber, and a vacuum for adjusting the pressure of the vacuum chamber. Pumps 5, 6, gauges 7 and 8 for measuring the degree of vacuum, power supplies 3 for generating potential differences in the electrodes, and non-reactive gases such as nitrogen and reactive gases around the sample to be surface treated. It consists of the reaction gas regulators 9, 10 etc. which are injected.

상기 장치에 의한 플라즈마중합처리의 일례를 설명하면 다음과 같다.An example of the plasma polymerization treatment by the above apparatus will be described.

챔버(1)에 시료(2)를 설치하고 로터리 펌프(5)를 기동하여 챔버 내부의 압력이 약 10-3Torr 정도의 진공으로 유지되는 것을 열전측정기(thermocouple gauge)(7)로 확인한 후, 확산펌프(6)를 기동시켜 챔버 내부의 압력이 10-6Torr 정도로 유지되는 것을 이온게이지(8)로 확인한다. 시료는 전원(3)에 의하여 애노드(또는 능동 전극)로 바이어스되어 위치하며, 반대쪽 전극(4)은 접지 되어 있다. 챔버의 압력이 일정 진공으로 유지되면 반응성 가스와 비반응성 가스를 원하는 위치 주위에 차례로 주입한다. 상기 가스의 혼합비는 열전측정기의 압력으로 조절한다. 진공 챔버 내의 압력이 일정 압력이 되면 직류 또는 고주파로 방전시킨다. 그러면 직류 또는 고주파에 의하여 발생된 플라즈마 내에서 상기 가스들의 분자 결합이 끊어지게 되고, 끊어진 체인과 활성화된 양이온이나 음이온들이 결합하여 전극 사이에 놓아둔 시료 표면에 중합물을 형성하게 된다.After installing the sample (2) in the chamber (1) and starting the rotary pump (5) to confirm that the pressure inside the chamber is maintained in a vacuum of about 10 -3 Torr by a thermocouple gauge (7), The diffusion pump 6 is started to confirm with the ion gauge 8 that the pressure inside the chamber is maintained at about 10 -6 Torr. The sample is positioned biased to the anode (or active electrode) by the power supply 3, and the opposite electrode 4 is grounded. When the pressure in the chamber is maintained at a constant vacuum, reactive and non-reactive gases are injected in turn around the desired location. The mixing ratio of the gas is controlled by the pressure of the thermoelectric meter. When the pressure in the vacuum chamber reaches a constant pressure, it is discharged by direct current or high frequency. Then, the molecular bonds of the gases are broken in the plasma generated by direct current or high frequency, and the broken chains and activated cations or anions combine to form a polymer on the sample surface placed between the electrodes.

그러나 상기 장치의 경우 연속처리가 불가능하여 생산성이 떨어진다. 반면에 도 2에 나타난 장치를 보면, 연속적으로 플라즈마중합 처리가 가능한 장치로서 특히 대면적의 시료를 박막 코팅시키는데 유리하다. 뿐만 아니라 시료의 양쪽 면에 대향전극이 배치되어 있어 동시에 중합이 가능하므로 생산성에 큰 효과를 가져오게 된다. 그러나 연속 장치에 있어서는 다음과 같은 문제점이 있다. 예를 들어 유기 모노머를 사용하여 증착되는 물질에 친수성을 가지는 유기막을 형성하고자 할 때, 상기 연속 장치의 경우 플라즈마 발생시 시료와 대향전극 사이의 거리에 따라 전압차이가 생기게 된다. 따라서 양면이 동일한 처리 효과를 가지기 위해서는 애노드와 캐소드 사이의 거리를 동일하게 할 필요가 있다. 그러나 플라즈마처리 전에 양 전극의 거리를 일정하게(도 2에서 시료와 각각의 대향전극과의 거리 A 및 B를 같게) 설정하였더라도 전극의 상태, 가스의 흐름, 압력 등에 따라 양 측의 전압이 달라질 수 있고, 이 경우 시료의 양면 처리 특성에 불균일을 가져올 수 있다. 특히 도 2에 나타난 것과 같이 연속적으로 장시간 플라즈마중합처리시에는 전극 양단의 특성 차이로 인하여 중합되는 물질의 불량을 일으킬 수 있다.However, in the case of the device, the continuous processing is not possible, so productivity is lowered. On the other hand, the apparatus shown in Fig. 2 is a device capable of continuously performing a plasma polymerization process, and is particularly advantageous for thin film coating a large-area sample. In addition, since the opposite electrodes are arranged on both sides of the sample, polymerization can be performed at the same time, which brings a great effect on productivity. However, in the continuous device, there are the following problems. For example, when forming an organic film having hydrophilicity on a material to be deposited using an organic monomer, in the case of the continuous device, a voltage difference occurs depending on the distance between the sample and the counter electrode during plasma generation. Therefore, in order for both surfaces to have the same treatment effect, it is necessary to make the distance between the anode and the cathode the same. However, even if the distance between the two electrodes is set before the plasma treatment (the distances A and B between the sample and each counter electrode are the same in FIG. 2), the voltage on both sides may vary according to the state of the electrodes, the flow of gas, and the pressure. In this case, non-uniformity may be brought about in the double-sided processing characteristics of the sample. In particular, as shown in FIG. 2, continuous plasma polymerization may cause a defect of a polymerized material due to a difference in characteristics at both ends of the electrode.

본 발명은 상기의 문제점을 해결하기 위한 것으로서, 연속적으로 플라즈마중합처리하는 경우에 시료와 시료의 양쪽면에 대향되는 각각의 대향전극 사이의 전압이 동일하도록 유지하는 수단을 구비함으로써 시료 양면이 동일하게 균일한 중합막이 형성되도록 하는 플라즈마중합 연속처리 장치를 제공함에 그 목적이 있다.SUMMARY OF THE INVENTION The present invention has been made to solve the above problems, and in the case of continuous plasma polymerization, both sides of the sample are equally provided by means for maintaining the same voltage between the sample and each counter electrode opposite to both sides of the sample. It is an object of the present invention to provide a plasma polymerization continuous processing apparatus for forming a uniform polymer film.

도 1은 종래기술에 의한 플라즈마중합처리장치를 나타내는 모식도이다.1 is a schematic diagram showing a plasma polymerization processing apparatus according to the prior art.

도 2는 연속적으로 플라즈마중합 처리가 가능한 장치의 일부를 나타내는 단면도이다.2 is a cross-sectional view showing a part of an apparatus capable of continuously performing plasma polymerization treatment.

도 3은 본 발명에 의한 일실시예로서, 전압조절부가 구비된 플라즈마중합 연속처리장치의 일부분을 나타내는 단면도이다.3 is a cross-sectional view showing a part of a plasma polymerization continuous processing apparatus provided with a voltage adjusting unit according to an embodiment of the present invention.

*** 도면의 주요 부분에 대한 부호의 설명 ****** Explanation of symbols for the main parts of the drawing ***

1:증착챔버 2:시료1: Deposition chamber 2: Sample

3:전원공급장치 4:대향전극3: power supply 4: counter electrode

5:로터리펌프 6:확산펌프5: rotary pump 6: diffusion pump

7:열전측정기 8:이온게이지7: Thermometer 8: Ion gauge

9:가스조절장치 10:가스조절장치9: gas regulator 10: gas regulator

20:풀림롤 21:풀림챔버20: unrolling roll 21: unwinding chamber

22:감김롤 23:감김챔버22: winding roll 23: winding chamber

30:고정거리캐소드 31:가변거리캐소드30: fixed distance cathode 31: variable distance cathode

33:고정거리캐소드전압부 34:가변거리캐소드전압부33: fixed distance cathode voltage section 34: variable distance cathode voltage section

36:전압차조정부 38:구동부36: voltage difference adjusting unit 38: driving unit

본 발명은 플라즈마중합 처리장치에 관한 것으로서, 상기의 문제점을 해결하기 위한 수단으로, 표면처리되는 시료를 풀어주어 다른 챔버로 이송시키는 풀림롤을 포함하는 풀림챔버와, 상기 풀림챔버의 풀림롤로부터 도입되는 시료의 상하에 대향되는 별도의 전극을 설치하며 상기 시료에 대향되는 각각의 대향전극과 시료 사이의 각각의 전압을 동일하게 유지시키기 위한 전압조절부를 구비하고 방전 플라즈마에 의해 상기 시료 양 표면 상을 플라즈마중합처리하는 증착챔버와, 상기 증착챔버에서 표면처리된 시료를 감아주는 감김롤을 포함하고 있는 감김챔버와, 상기 증착챔버를 진공으로 유지하기 위한 펌핑수단 및 반응성 가스 및 비반응성 가스를 도입하는 가스유입구를 포함하여 구성되는 플라즈마중합 연속처리장치를 제공한다.The present invention relates to a plasma polymerization apparatus, which is a means for solving the above problems, which is introduced from an unwinding chamber including a unwinding roll for releasing a surface-treated sample and transferring it to another chamber, and the unrolling roll of the unwinding chamber. A separate electrode facing each other above and below the sample is provided, and a voltage adjusting unit for maintaining the same voltage between each counter electrode facing the sample and the sample is the same. A deposition chamber including a deposition chamber for performing plasma polymerization, a winding roll for winding a surface treated sample in the deposition chamber, pumping means for maintaining the deposition chamber under vacuum, and introducing a reactive gas and a non-reactive gas; Provided is a plasma polymerization continuous processing apparatus including a gas inlet.

본 발명은 종래 기술에서 플라즈마 처리 중 시료의 양면에서 전압의 불균일이 발생할 수 있는 문제점을 해결하기 위하여 일측의 대향전극은 고정시켜 시료와의 거리를 항상 일정하게 하고, 다른 일측의 대향전극은 시료와의 거리를 가변시킬 수 있도록 한 것을 특징으로 한다.The present invention in order to solve the problem that the voltage non-uniformity may occur on both sides of the sample during the plasma treatment in the prior art, the one side of the counter electrode is fixed to always keep the distance from the sample, the other side of the counter electrode Characterized in that the distance can be varied.

상기의 본 발명을 실시하기 위한 구체적인 수단으로서 상기 전압조절부는 시료와 상기 시료에 대향되는 각각의 대향전극 사이에 작용하는 전압을 측정하는 전압측정장치와, 시료와 각 대향전극 사이에 인가되는 양측의 전압차를 계산하고 이 전압차에 해당하는 신호를 발생시켜 외부로 전달하는 전압차조정부 및 상기 전달된 신호를 받고 이 신호에 의해 회전함으로써 대향전극의 위치를 이동시키는 구동부로 구성된다.As a specific means for carrying out the present invention, the voltage adjusting unit includes a voltage measuring device for measuring a voltage acting between a sample and each counter electrode facing the sample, and a voltage measuring device for measuring the voltage applied between the sample and each counter electrode. Comprising a voltage difference adjusting unit for calculating a voltage difference and generating a signal corresponding to the voltage difference and transmitting it to the outside, and a drive unit for receiving the transmitted signal and rotating by the signal to move the position of the counter electrode.

도 3에 본 발명의 구체적인 실시예로서, 플라즈마중합 연속처리장치의 일부분이 나타나 있다. 본 발명에 의한 전압조절 과정을 살펴보면 다음과 같다. 도 3에 나타난 바와 같이 시료(2)에 연속적으로 플라즈마 중합처리를 하는 장치에 있어서 플라즈마 처리 전에는 두 캐소드(30, 31)와 애노드로 사용되는 시료(2) 사이의 거리를 같게 맞추어 놓는다. 플라즈마 발생 후의 중합처리 과정에서는 두 캐소드와 애노드 사이에 걸리는 각각의 인가 전압을 전압측정부에서 측정한다. 즉, 고정거리 캐소드(30)는 고정거리 캐소드 전압부(33)에서, 가변거리 캐소드(31)는 가변거리 캐소드 전압부(34)에서 각각 측정한다. 그 다음에는 상기의 각 측정 전압을 전압차 조정부(36)에서 계산하고, 이 때 각 전압 사이에 차이가 발생하면 구동부(38)에 신호를 보내어 구동부의 회전에 의해 가변측 캐소드의 위치를 조정하여 고정측의 전압과 같아질 때까지 이동시킨다. 거리의 가변 방법은 작업자가 수동으로 이동시킬 수도 있고, 모터나 공기압 등을 이용하여 자동적인 제어에 의해 움직일 수 있다.As a specific embodiment of the present invention in Fig. 3, a part of the plasma polymerization continuous processing apparatus is shown. Looking at the voltage regulation process according to the present invention. As shown in Fig. 3, in the apparatus for continuously plasma-polymerizing the sample 2, the distance between the two cathodes 30 and 31 and the sample 2 used as the anode is equalized before the plasma treatment. In the polymerization process after plasma generation, the voltage applied to each of the applied voltages between the two cathodes and the anode is measured. That is, the fixed distance cathode 30 is measured by the fixed distance cathode voltage unit 33 and the variable distance cathode 31 is measured by the variable distance cathode voltage unit 34, respectively. Then, the above-described measured voltages are calculated by the voltage difference adjusting unit 36. At this time, if a difference occurs between the voltages, a signal is sent to the driving unit 38 to adjust the position of the variable side cathode by the rotation of the driving unit. Move until it is equal to the voltage on the fixed side. The method of varying the distance can be moved manually by an operator or can be moved by automatic control using a motor or air pressure.

따라서 플라즈마중합 연속처리시에 장시간 작업을 수행하는 동안 전극의 상태, 가스의 흐름, 압력의 변화 등으로 시료 양측의 전압이 불균일하게 되더라도 상기와 같은 가변전극에 의하여 가변측 캐소드와 시료 사이의 전압을 고정측 캐소드와 시료 사이의 전압과 일정하도록 유지시킬 수 있다.Therefore, even if the voltage on both sides of the sample becomes uneven due to the state of the electrode, the flow of gas, the pressure change, etc. during the long time operation during the plasma polymerization continuous process, the voltage between the variable cathode and the sample is controlled by the variable electrode as described above. It can be kept constant with the voltage between the fixed side cathode and the sample.

본 발명에 의하면 종래 연속적으로 플라즈마중합처리하는 장치에 시료와 시료의 양 쪽면에 대향되는 각각의 대향전극 사이의 전압이 동일하도록 유지하는 수단으로 전압조절부를 구비함으로써, 전극의 상태, 가스의 흐름, 압력의 변화 등으로 시료 양측의 전압이 불균일하게 되더라도 가변전극에 의하여 가변측 대향전극과 시료 사이의 전압을 고정측 대향전극과 시료 사이의 전압과 동일하도록 유지시킬 수 있으므로 시료 양면이 동일하게 균일한 중합막이 형성되도록 할 수 있으며, 따라서 신뢰성 있는 중합막을 형성하는 플라즈마중합 연속처리 장치를 제공할 수 있다.According to the present invention, the apparatus for continuously performing the plasma polymerization process includes a voltage adjusting unit as a means for maintaining the same voltage between the sample and each counter electrode opposite to both sides of the sample, so that the state of the electrode, the flow of gas, Even if the voltage on both sides of the sample becomes uneven due to a change in pressure, the voltage between the variable side counter electrode and the sample can be maintained to be the same as the voltage between the fixed side counter electrode and the sample by the variable electrode. The polymerized film can be formed, and therefore, a plasma polymerization continuous processing apparatus for forming a reliable polymerized film can be provided.

Claims (1)

표면처리되는 시료를 풀어주어 다른 챔버로 이송시키는 풀림롤을 포함하는 풀림챔버와,An unwinding chamber including a unwinding roll for releasing the surface treated sample and transferring it to another chamber; 상기 풀림챔버의 풀림롤로부터 도입되는 시료의 상하에 대향되는 별도의 대향전극을 설치하며, 상기 시료에 대향되는 각각의 대향전극과 시료 사이의 각각의 전압을 동일하게 유지시키기 위한 전압조절부를 구비하고, 플라즈마에 의해 상기 시료 양 표면 상을 플라즈마중합처리하는 증착챔버와,It is provided with a separate counter electrode facing the upper and lower sides of the sample introduced from the unwinding roll of the unwinding chamber, and provided with a voltage control unit for maintaining the same voltage between each counter electrode and the sample facing the sample A deposition chamber for performing plasma polymerization on both surfaces of the sample by plasma; 상기 증착챔버에서 표면처리된 시료를 감아주는 감김롤을 포함하고 있는 감김챔버와,A winding chamber including a winding roll for winding a sample treated in the deposition chamber; 상기 증착챔버를 진공으로 유지하기 위한 펌핑수단 및Pumping means for maintaining the deposition chamber in vacuum; 반응성 가스 및 비반응성 가스를 도입하는 가스유입구를 포함하여 구성되는 플라즈마중합 연속처리장치.A plasma polymerization continuous processing apparatus comprising a gas inlet for introducing a reactive gas and a non-reactive gas.
KR1019990035224A 1999-08-24 1999-08-24 An apparatus for forming polymer continuously on the surface of metal by dc plasma polymerization KR20010019025A (en)

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Publication number Priority date Publication date Assignee Title
US9297075B2 (en) 2011-08-30 2016-03-29 Mitsubishi Electric Corporation Plasma deposition apparatus and plasma deposition method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9297075B2 (en) 2011-08-30 2016-03-29 Mitsubishi Electric Corporation Plasma deposition apparatus and plasma deposition method

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