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WO2010058648A1 - Procédé de modification de surface utilisant un micro-plasma et procédé de liaison utilisant un micro-plasma - Google Patents

Procédé de modification de surface utilisant un micro-plasma et procédé de liaison utilisant un micro-plasma Download PDF

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Publication number
WO2010058648A1
WO2010058648A1 PCT/JP2009/065986 JP2009065986W WO2010058648A1 WO 2010058648 A1 WO2010058648 A1 WO 2010058648A1 JP 2009065986 W JP2009065986 W JP 2009065986W WO 2010058648 A1 WO2010058648 A1 WO 2010058648A1
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Prior art keywords
microplasma
surface modification
electrode
modification treatment
processed
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English (en)
Japanese (ja)
Inventor
清水一男
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Yodogawa Hu Tech Co Ltd
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Yodogawa Hu Tech Co Ltd
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    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
    • H05H1/00—Generating plasma; Handling plasma
    • H05H1/24—Generating plasma
    • H05H1/2406—Generating plasma using dielectric barrier discharges, i.e. with a dielectric interposed between the electrodes
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
    • H05H1/00—Generating plasma; Handling plasma
    • H05H1/24—Generating plasma
    • H05H1/2406—Generating plasma using dielectric barrier discharges, i.e. with a dielectric interposed between the electrodes
    • H05H1/2418—Generating plasma using dielectric barrier discharges, i.e. with a dielectric interposed between the electrodes the electrodes being embedded in the dielectric
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
    • H05H1/00—Generating plasma; Handling plasma
    • H05H1/24—Generating plasma
    • H05H1/2406—Generating plasma using dielectric barrier discharges, i.e. with a dielectric interposed between the electrodes
    • H05H1/2437—Multilayer systems

Definitions

  • the present invention relates to a surface modification method using microplasma and a bonding method using microplasma.
  • Patent Document 1 In the surface modification process by the conventional method as described above, a high voltage power source is required for plasma generation (usually 10-20 kV for the surface modification process) as well as the cost of the robot control part.
  • Non-Patent Document 1, Patent Document 2, and Patent Document 3 Regarding the surface modification processing technology, there are the following demands from the industry. (1) In the liquid crystal industry where competition for real-time processing is extremely fierce, speed processing is required, and it is difficult to deal with decompression processing that requires a vacuum chamber or the like, and an atmospheric pressure process capable of simple and large-area processing is required. It has become.
  • micro flow path having an extremely small cross-sectional area is driven by a high pressure pump or the like, it is required to improve the bonding strength.
  • (4) Adverse effects of electrostatic damage When corona discharge or glow discharge treatment is performed, charging of the material to be treated by charged particles becomes a problem.
  • the liquid crystal panel has an adverse effect on mounted parts, formation lines, and the like, and is considered to be a cause of inefficient surface modification.
  • microplasma Compared with atmospheric pressure corona and glow discharge, microplasma has a discharge voltage of about 1/10 (1 kV), and since the material to be treated is placed outside, the corona often sandwiches the material to be treated between the electrodes. It is considered that adverse effects are less likely to be seen compared to discharge treatment or the like.
  • Patent Document 4 describes a “microreactor” in which two substrates are bonded with an adhesive and a microchannel recess having a width of 0.1 to 3000 ⁇ m is formed at the interface between the substrates.
  • a solvent or an adhesive may be mixed in the chemical solution of the contents.
  • An object of the present invention is to provide a method for modifying the surface characteristics of various materials such as glass and resins to a large area in real time using atmospheric pressure microplasma.
  • Another object of the present invention is a method of joining a member to be treated such as a plurality of flexible members by heating and pressurizing without using an adhesive.
  • the object is to provide a method for joining a member to be processed which has no fear of mixing with a solvent, an adhesive or the like and has excellent joining durability.
  • the surface modification method using the microplasma of the present invention is as follows: Atmospheric pressure microplasma generated between a plurality of microplasma electrodes at 780 V to 1.9 kV under atmospheric pressure is irradiated onto the surface of the member to be processed, and the surface modification treatment of the surface of the member to be processed is performed without using a vacuum vessel. In real time.
  • the surface modification treatment method using the microplasma of the present invention is the above (1).
  • the atmospheric pressure microplasma is generated at 780 V to 1 kV so that static electricity is not generated in the member to be processed.
  • the surface modification treatment method using the microplasma of the present invention is the above (1) or (2).
  • the surface modification treatment method using microplasma of the present invention is the above (3).
  • the hole formed in the microplasma electrode has a diameter of 0.5-5 mm.
  • the surface modification treatment method using microplasma of the present invention is any one of the above (1) to (4),
  • the flow rate of the gas injected from the hole formed in the microplasma electrode is 1 to 5.5 m / s.
  • the surface modification treatment method using the microplasma of the present invention is any one of the above (1) to (5).
  • the distance between the microplasma electrode and the surface of the member to be processed is set to 0 to 10 mm.
  • the surface modification treatment method using microplasma of the present invention is any one of the above (1) to (6),
  • the discharge gap length between the microplasma electrodes is set to 0 to 500 ⁇ m.
  • the surface modification treatment method using the microplasma of the present invention is any one of the above (1) to (7).
  • the entire surface of the microplasma electrode is used to perform a surface modification process on the surface of the member to be processed.
  • the surface modification treatment method using microplasma of the present invention is any one of the above (1) to (8), In setting the discharge gap between the microplasma electrodes, Without using a separate spacer, a dielectric is coated on the surface of the microplasma electrode to ensure a discharge gap length.
  • a joining method using microplasma of the present invention is a joining method of a member to be processed whose surface has been modified by using the surface modification treatment method according to any one of (1) to (9). And It is characterized in that the surfaces of the treated members subjected to the surface modification treatment are heated and pressurized to be joined without using an adhesive.
  • microplasma of the present invention physical changes and chemical changes caused by generated radicals, ultraviolet light, etc. are caused by performing microplasma treatment on the surface of the member to be treated.
  • it is possible to perform a surface modification process for a large area in real time without the need for a vacuum vessel such as a chamber.
  • it can be handled with a small power source, and atmospheric gas can be used, which is advantageous in terms of cost.
  • surface modification treatment that does not adversely affect electrostatic damage is possible. That is, when corona discharge or glow discharge treatment is performed, charging of the member to be treated by charged particles becomes a problem.
  • the liquid crystal panel has an adverse effect on mounted components, formation lines, and the like, and is considered to be a cause of inefficient surface modification.
  • the discharge voltage is about 1/10 (1 kV)
  • the member to be processed is placed outside, the member to be processed is often sandwiched between the electrodes.
  • corona discharge treatment there are few adverse effects.
  • the bonding method using the microplasma of the present invention since the processing target members are bonded without using an adhesive, there is no possibility that the adhesive component is eluted into the contents, and the influence on the contents There is no.
  • the present invention can be preferably applied when the content is food, medicine or the like.
  • the members to be processed are joined by heating and pressing, the members to be processed can be integrated by a simple means and can be preferably applied to a liquid container or the like.
  • the member to be treated is a resin film
  • the resin film is heated evenly, so that peeling is unlikely to occur on the bonding surface between the films.
  • FIG. 1 is a schematic configuration of a plasma electrode used for microplasma processing, where (a) is a cross-sectional view of the plasma electrode, and (b) is a plan view of the plasma electrode.
  • FIG. 2 is an explanatory view of a method for joining processed members using the microplasma processing of the present invention.
  • FIG. 3 is a photograph of the contact angle measured in order to evaluate the effect of the surface modification treatment.
  • FIG. 4 shows an example of the result of microplasma surface modification treatment with a PEN film (polyethylene naphthalate) in Example 2, where (1) is untreated (2) is treated with an applied voltage of 780 V, and (3) is 880 V. (4) is processed at 1 kV.
  • FIG. 1 is a schematic configuration of a plasma electrode used for microplasma processing, where (a) is a cross-sectional view of the plasma electrode, and (b) is a plan view of the plasma electrode.
  • FIG. 2 is an explanatory view of a method for joining processed members using the microplasm
  • FIG. 5 shows the result of a water droplet contact angle change on the glass substrate when the surface of the glass substrate in Example 3 was subjected to microplasma surface modification treatment.
  • FIG. 6 shows the results of changes in the contact angle of water droplets on the surface of the LCP when the surface of the LCP (Liquid Crystal Polymer: liquid crystal polymer) of Example 4 was subjected to microplasma surface modification treatment.
  • FIG. 7 shows the result of a change in water droplet contact angle on the surface of PPA when the surface of PPA (polyphthalamide) in Example 5 was subjected to microplasma surface modification treatment.
  • FIG. 8 shows the result of the water droplet contact angle change on the surface of the lead frame in Example 6.
  • FIG. 9 shows the result of the water droplet contact angle change on the surface of the PC in Example 7.
  • FIG. 10 shows the adhesion between LCP and silicon after 48 hours in Example 8.
  • FIG. 11 shows the adhesion between LCP and silicon after 72 hours.
  • FIG. 12 shows the adhesion between LCP and silicon after 120 hours.
  • FIG. 13 shows the measurement result of the contact angle in this case, in which the surface modification treatment of the member to be treated was performed by changing the through-hole diameter of the plasma electrode.
  • FIG. 14 shows the influence of Example 10 on the contact angle of the PEN film surface when the gas flow rate was changed.
  • FIG. 15 shows the relationship of the distance between the electrode (dielectric part) and the member to be processed in microplasma processing in Example 11.
  • FIG. 16 shows the change in the contact angle depending on the treatment time when argon is used as the rare gas for the surface modification treatment of the PEN film in Example 12.
  • FIG. 17 shows the influence of the injection gas type on the contact angle in Example 13.
  • 18A shows a microplasma experimental apparatus diagram of Example 15, and
  • FIG. 18B shows a corona discharge experimental apparatus diagram of Comparative Example 1.
  • FIG. FIG. 19 shows the experimental results of FIG.
  • FIG. 20 shows the change in the C1s spectrum on the surface of the PEN film before and after performing microplasma treatment using Ar gas as the injection gas in Example 16.
  • FIG. 21 shows the O1s spectrum on the surface of the PEN film before treatment in Example 16 and the change in the O1s spectrum on the surface of the PEN film when treated with Ar.
  • FIG. 22 shows the N1s spectrum on the surface of the PEN film before the treatment in Example 16 and the N1s spectrum change on the surface of the PEN film when treated with Ar.
  • FIG. 23 shows an electrode temperature distribution in Example 17 when the area of the plasma electrode is 20 ⁇ 100 mm 2 .
  • FIG. 24 shows an electrode temperature distribution in Example 17 when the area of the plasma electrode is 60 ⁇ 100 mm 2 .
  • FIG. 25 shows an electrode temperature distribution in Example 17 when the area of the plasma electrode is 100 ⁇ 100 mm 2 .
  • FIG. 26 shows an example in which the resin coating of Example 18 was provided with a difference in thickness and a discharge gap length of 100 ⁇ m was formed on the electrode surface.
  • FIG. 27 is an explanatory diagram for forming a fluid manifold made of the three-layer resin film of Example 19.
  • FIG. 28 shows the result of analyzing the bonding state with a laser focus microscope.
  • a film to be activated (member to be treated) is installed below an electrode for generating microplasma, and an alternating voltage is applied to the upper microplasma electrode.
  • the microplasma used in the present invention can be driven with a Paschen minimum of about 10 ⁇ m at atmospheric pressure, and thus is essentially characterized by extremely high energy efficiency (active species generation efficiency in plasma).
  • the member to be treated by the surface modification treatment method of the present invention is not particularly limited as long as it is a dielectric, but polyester, polyethylene terephthalate, polycarbonate, polypropylene, polymethylpentene, polychlorinated Examples thereof include resin films made from vinyl, polyurethane, and the like.
  • the resin film may be a single layer or a laminated layer.
  • the resin film excellent in chemical resistance and heat resistance include polyethylene naphthalate (PEN), polyimide (PI), and polyetheretherketone (PEEK).
  • PEN polyethylene naphthalate
  • PI polyimide
  • PEEK polyetheretherketone
  • the target of the surface modification by the surface modification treatment method of the present invention can be applied to a resin substrate, a glass substrate, and other substrates in addition to the resin film, and is not particularly limited.
  • a schematic configuration of a plasma electrode used for the microplasma treatment is shown in FIG. 1A is a cross-sectional view of a plasma electrode, and FIG. 1B is a plan view of the plasma electrode.
  • the plasma electrode 10 includes two metal substrates 13 each having a plurality of through holes 11 arranged in parallel.
  • the plasma electrodes 10 are arranged in parallel at the peripheral portion with a non-conductive spacer 15 interposed therebetween. Furthermore, a dielectric film 16 is formed on the surface of the metal substrate 13, and the surface of the dielectric film 16 is preferably an uneven shape with a porous surface exposed. Furthermore, a ground electrode 18 is provided under the member 17 to be processed (resin film, glass substrate, resin substrate, etc., which is the target of surface modification), and charged particles such as ions are actively applied to the surface of the member 17 to be processed. By supplying to the surface treatment, the surface treatment can be accelerated.
  • the distance between workpieces of the member 17 to be processed and the metal substrate 13 having the dielectric film 16 is within 0-5 mm.
  • CDA Clean dry air
  • rare gases such as nitrogen and argon are injected through the through-hole 11 provided in the plasma electrode 10
  • the injection gas flow rate from the through hole 11 of the plasma electrode 10 to the member 17 to be processed is about 1 to 5.5 m / s.
  • the discharge gap length which is the plasma generation region between the microplasma electrodes, is preferably set between 0-500 ⁇ m, and more preferably between 0-300 ⁇ m.
  • the plasma electrode 10 desirably has a plurality of through holes 11 formed therein.
  • the total opening area ratio of the opening portions of the through holes 11 formed in the metal substrate 13 is 2-60% with respect to the plane area when the metal substrate 13 is viewed from the plane. Is preferred.
  • the discharge gap length which is the plasma generation region between the microplasma electrodes
  • the size of the through hole 11 is preferably 0.5-5 mm in order to ensure that the injection gas flow rate is 1-5.5 m / s.
  • the peak value of the voltage is about 500V-2kV, and plasma can be generated at atmospheric pressure.
  • the range is preferably 700V-1.5kV.
  • the average current depends on the area of the electrode, but is preferably in the range of about 20 mA-10 A.
  • the frequency of the power source may be any band in the region from a low frequency to a very high frequency in the range of 1 kHz to 1000 MHz, but a frequency in the range of about 10 kHz to 100 kHz is preferable in consideration of an increase in electrode temperature.
  • the heating temperature of the plasma electrode 10 is preferably room temperature-300 ° C., more preferably in the range of room temperature-100 ° C.
  • a method for joining processed members using microplasma processing is a method in which a plurality of processed members are joined by heating and pressing without using an adhesive, and the processed member is formed by microplasma. It processes, after that, to-be-processed members are heated and pressurized, and to-be-processed members are joined. As shown in FIG. 2, the activated surfaces of the two processed members 2 and 3 that have been subjected to surface modification treatment by plasma treatment face each other and are placed on the lower press die 21. Further, the upper press die 22 heated by the external heating device (heater) 23 is placed in a standby state above the members 2 and 3 to be processed.
  • the two processed members 2 and 3 disposed on the lower press mold 21 are pressed by the heated upper press mold 22 to join the processed members 2 and 3 together.
  • the heating temperature of the press upper die 22 needs to be a temperature that softens the member to be processed, it is preferable that the temperature of the softening point is slightly lower than the melting point of the member to be processed.
  • the melting point is 265-270 ° C.
  • the heating temperature by the heater is preferably about 145-147 ° C.
  • the heating temperature by the heater is preferably about 230 to 250 ° C.
  • the applied pressure at the time of joining is such that the member to be treated is softened and sufficient joining strength is obtained. If a further pressing force is applied, the member to be processed is destroyed, so that the thickness is adjusted as appropriate according to the thickness of the material to be processed. For example, when joining at the softening point using PEN as a member to be treated, it is sufficient to set the pressure to about 1-3 Pa (10-30 kgf / cm 2 ).
  • Example 1 The surface of the PEN film using a disk-shaped plasma electrode made of 18-8 stainless steel with a thickness of 0.5 mm and an outer diameter of 100 mm formed of a metal substrate punched with a large number of circular through-holes. A reforming treatment was performed. The through hole formed in the metal substrate had an outer diameter of one through hole of 0.2 mm and an opening area ratio of 50%. A dielectric material was coated on the surface of the metal substrate 13. The dielectric film is preferably coated with a ceramic coating such as glass coating or alumina, or with another ceramic or insulating material. As a voltage driving condition, a voltage of 920 V was applied between the plasma electrode 10 and the ground electrode 18 to drive, thereby generating plasma in a silent discharge state.
  • a voltage driving condition a voltage of 920 V was applied between the plasma electrode 10 and the ground electrode 18 to drive, thereby generating plasma in a silent discharge state.
  • the PEN film was subjected to surface modification by flowing a gas vertically through the through hole of the metal substrate to generate microplasma between the plasma electrodes.
  • the conditions for surface modification were as follows.
  • the injection gas flow rate was 1 L / min, and the processing time was 10 min.
  • As the kind of gas pure air and nitrogen were used.
  • the contact angle (side view) to the film was photographed. The photograph is shown to FIG. 3 (1)-(4).
  • the contact angle ⁇ is obtained from the calculation formula shown in Table 1, and the result is shown in Table 1.
  • the contact angle before the modification was 86.9 °, but by the surface modification treatment of the present invention, the contact angle was as follows.
  • the contact angle after modification is 60.3 °
  • the contact angle after modification is 60.2 °
  • the contact angle after modification is 54.2 °
  • the contact angle after modification is 22.3 °
  • Example 2 shows the dependency of the applied voltage in the microplasma surface modification treatment.
  • the applied voltage was changed to 780 V, 880 V, and 1 kV under the conditions of argon as the injection gas, a gas flow rate of 10 L / min, and a processing time of 1 min.
  • the discharge gap length between the electrodes was 300 ⁇ m.
  • a PEN film was used as a member to be treated for the microplasma surface modification treatment, and the water droplet contact angle on the film surface was measured and evaluated.
  • Example 3 a glass substrate as a substrate used in a liquid crystal panel or the like was used as the member to be processed.
  • the surface of the glass substrate is subjected to microplasma surface modification treatment, and the result of the water droplet contact angle change on the glass substrate is shown in FIG. Table 3 summarizes the experimental parameters in this case. From the results of FIG. 5, the water droplet contact angle on the glass substrate before the surface modification treatment using microplasma was 39-43 °, but after the surface modification treatment, the water droplet contact angle was greatly reduced.
  • Example 4 LCP was used as the member to be processed. The surface of the LCP is subjected to a microplasma surface modification treatment, and the result of the water droplet contact angle change on the surface of the LCP is shown in FIG. Table 4 summarizes the experimental parameters.
  • Example 5 In Example 5, PPA (polyphthalamide) was used as the member to be treated. The experimental parameters are the same as in Table 4 shown in Example 4.
  • Example 6 The surface of PPA (polyphthalamide) is subjected to microplasma surface modification treatment, and the result of the water droplet contact angle change on the surface of PPA is shown in FIG. (Example 6)
  • the lead frame metal plate used at the time of semiconductor manufacture was used as a member to be processed.
  • the surface of the lead frame is subjected to AG plating and Pd plating.
  • the experimental parameters are the same as in Table 4 shown in Example 4.
  • FIG. 8 shows the results of changes in the contact angle of water droplets on the surface of the lead frame when the surface of the lead frame was subjected to microplasma surface modification treatment.
  • PC polycarbonate
  • Example 8 The experimental parameters are the same as in Table 4 shown in Example 4.
  • the surface of PC polycarbonate
  • FIG. Example 8
  • the results of observing the sustainability after performing the microplasma treatment for 30 seconds on the adhesion (adhesiveness or bondability) between the LCP and silicon as the member to be treated are shown in FIGS. .
  • 10 shows adhesion between LCP and silicon after 48 hours
  • FIG. 11 shows adhesion between LCP and silicon after 72 hours
  • FIG. 12 shows adhesion between LCP and silicon after 120 hours. Observed.
  • FIG. 10 shows adhesion between LCP and silicon after 48 hours
  • FIG. 11 shows adhesion between LCP and silicon after 72 hours
  • FIG. 12 shows adhesion between LCP and silicon after 120 hours.
  • Example 9 In Example 9, the diameter of the through hole 11 of the plasma electrode is changed to perform the surface modification treatment of the member 17 to be processed, and the contact angle measurement result in this case is shown in FIG. In addition, the to-be-processed material 17 used the glass base material, and the water droplet contact angle before a process was about 25 degree
  • the contact angle change is small for the diameter of the through-hole 11 of 5 mm depending on the microplasma processing time (reduction of 6.9 ° in the processing time of 60 seconds), the diameter of the through-hole 11 is small.
  • the contact angle became less than the measurement limit at a processing time of 60 seconds.
  • the contact angle decreased to 10 ° even with a treatment time of 5 seconds.
  • the gas flow rates in the through holes 11 are summarized in Table 5. As shown in Example 6, the gas flow rate shows an optimum value at 1 [m / s] or more, and when the gas flow rate is further increased, it tends to decrease again.
  • FIG. 14 shows the influence on the contact angle of the PEN film surface when the gas flow rate is changed in Example 10.
  • the injection gas used for the surface modification treatment of the PEN film was air, and was supplied to the microplasma electrode using a fan.
  • the discharge gap length of the microplasma electrode is 100 ⁇ m, and the applied voltage is 1.5 kV.
  • the member to be processed has a contact angle once reduced at an injection gas flow rate of 3.0 m / s, and that the contact angle increases as the flow rate increases from there.
  • Example 11 In Example 11, the relationship between the distance between the electrode (dielectric part 16) and the member to be processed 17 in the microplasma processing is shown in FIG.
  • the to-be-processed member 17 uses the glass base material, and the water droplet contact angle before a process is about 30 degree
  • the distance between the electrode (dielectric part 16) and the member to be processed 17 is 10 mm, the effect of the surface modification treatment is small, and the electrode (dielectric part 16) and the member to be processed 17 When the distance is shortened, the contact angle is decreased, and the effect of the surface modification treatment is greatly exhibited. In particular, when the distance between the member to be processed and the electrode was 5 mm or less, the contact angle was below the measurement limit.
  • Example 12 In Example 12, the change in the contact angle depending on the treatment time when argon is used as the rare gas for the surface modification treatment of the PEN film is shown. In Example 1, the result of processing for about 10 minutes using nitrogen and room air was shown. However, in Example 12, since argon was used, the PEN film contacted in about 3 seconds as shown in FIG. The angle decreased to about 30 degrees and the hydrophilicity increased. Even if the treatment time is further increased, the contact angle does not change greatly, so that the effectiveness of using a rare gas for shortening the treatment time is recognized.
  • Example 12 the interelectrode discharge gap length was 100 ⁇ m, the distance between the PEN and the electrode was 1 mm, the discharge voltage was 1.1 kV, the discharge current was 28 mA, and the gas flow rate was 3.5 m / s.
  • Example 13 the influence on the contact angle when nitrogen or argon is added to room air as the propellant gas is shown.
  • FIG. 17 shows the results of comparing changes in the contact angle on the PEN surface using the following three types of propellant gas.
  • Example 14 When treated with nitrogen alone, it was 65.2 °.
  • an LCD panel substrate was used as the member to be processed.
  • the charging voltage of the LCD panel substrate after the surface modification treatment using microplasma was measured, and the influence of static electricity was evaluated.
  • the measuring instrument used was made by Static Sensor Model 718, 3M.
  • the conditions at the time of measurement are as follows. Gas type: nitrogen 70 L / min, discharge voltage: 1 KV, through-hole diameter: 2 mm, distance between electrode (dielectric part) and member to be processed: 3 mm
  • Table 10 shows the measurement results. There was almost no effect on the LCD panel substrate after the microplasma treatment, and the phenomenon that the bare chip on the LCD panel was destroyed by electrostatic failure was not observed.
  • Table 11 shows performance evaluation data of a static eliminator (ionizer) on an LCD panel.
  • the LCD panel was triboelectrically charged only by being transported on the production line, and voltages up to 68-155V were observed.
  • the charging voltage of the panel is standardized to be ⁇ 50 V or less. Even in comparison with these, since the voltage rises to only 30 V even after 60 seconds of microplasma treatment, the chips reported in the prior art (plasma surface treatment) are not damaged due to electrostatic failure, It can be said that the microplasma treatment has almost no influence of static electricity. Electrically, the lines of electric force are closed between the electrodes.
  • Example 15 Comparative Example 1
  • a plasma electrode having a hole diameter of 3 mm was used, the discharge gap length was 100 ⁇ m, and the distance between the member to be treated (PEN film) and the electrode was 1 mm, 2 mm, and 3 mm.
  • the surface modification treatment of the PEN film was performed for 5 seconds at an input voltage of 100 V, a discharge voltage of 1.9 kV, a discharge current of about 120 mA, and a room air (5 L / min).
  • the surface treatment by corona discharge was performed with a distance between the PEN film and the electrode of about 0.5 mm, a discharge voltage of 2.5 kV, a discharge current of about 180 mA, a room air (5 L / min), and a treatment time of 5 seconds. Under each condition, the surface potential was measured using a surface potentiometer (Trek, Model 347) after the surface treatment.
  • An experimental apparatus is shown in FIG. In FIG. 18, (a) shows a microplasma experimental apparatus, and (b) shows a corona discharge experimental apparatus. The experimental results are shown in FIG. From FIG. 19, when the microplasma electrode was used, the surface potential tended to decrease as the distance from the electrode to PEN increased.
  • Example 16 when the microplasma treatment is performed on the surface of the PEN film as the member to be treated, the change in chemical bonding on the surface is analyzed using XPS.
  • FIG. 20 shows the change in the C1s spectrum on the surface of the PEN film before and after performing the microplasma treatment using Ar gas as the injection gas. From FIG. 20, this spectrum shows C—H bonds, and it can be confirmed that C—H bonds are reduced by the microplasma treatment.
  • Example 17 in order to demonstrate that it is preferable to increase the area of the plasma electrode in the surface modification treatment using microplasma, plasma electrodes having various areas were manufactured and verified. In the present example, the surface temperature of the plasma electrode was observed with a thermo camera. However, since the electrode surface temperature rises when the plasma generation density is high, this measurement result suggests the plasma generation density.
  • FIG. 23 shows the electrode temperature distribution when the area of the plasma electrode is 20 ⁇ 100 mm 2 . As can be seen from FIG.
  • FIG. 24 shows the electrode temperature distribution when the area of the plasma electrode is 60 ⁇ 100 mm 2 . As can be seen from FIG. 24, it was recognized that the plasma generation was uneven in the 60 ⁇ 100 mm 2 electrode. From this result, it is understood that the surface modification may be limited to a certain area of the electrode area when the fixing method is not devised or when the thickness of the material (base material) is thin.
  • FIG. 25 shows an electrode temperature distribution when the area of the plasma electrode is 100 ⁇ 100 mm 2 . As can be seen from FIG. 25, it was recognized that the plasma generation was uneven in the 100 ⁇ 100 mm 2 electrode.
  • the plasma generation density around the clip for fixing the electrode is high.
  • these are considered to be improved by improving electrode processing accuracy (for example, setting of the discharge gap length, electrode fixing method, and power source capacity).
  • Example 18 In FIG. 1, the discharge gap length of 100 ⁇ m is secured by sandwiching the spacers between the electrodes.
  • the metal substrate constituting the plasma electrode is formed.
  • Example 26 shows an example in which a difference in thickness (step) is provided in the resin coating and a discharge gap length is formed on the electrode surface.
  • the electrode (a) portion (1): 350 ⁇ m, (2): 250 ⁇ m,
  • the electrode (b) part (2): 250 ⁇ m, (3): 350 ⁇ m.
  • Example 19 In Example 19, using the same apparatus as in Example 1, as shown in FIG. 27 (a), the member to be treated 4 is made of three resin films 2, 3, and 4 without using an adhesive. Bonding was performed by heating and pressing to form a fluid manifold made of three layers of resin film. In addition, about the resin film 3, both surfaces were surface-modified (activation process). In Example 19, the resin film 3 formed with the slits 5 as shown in FIG.
  • FIGS. 28 (a) and 28 (b) show the result of analyzing the bonding state with a laser focus microscope. The sample shown in FIG.
  • the surface modification treatment method using microplasma of the present invention causes the chamber to undergo physical changes and chemical changes caused by radicals generated by atmospheric pressure microplasma treatment, ultraviolet light, etc. on the surface of the member to be treated. It is possible to perform surface treatment over a large area in real time without the need for a vacuum vessel, etc., and it can be handled with a small power source, etc., and does not use expensive rare gas or standard gas, It can be diverted, is advantageous in terms of cost, and has high industrial applicability. Furthermore, since surface modification treatment that does not adversely affect electrostatic damage is possible, surface modification of a liquid crystal panel or the like can be performed with high efficiency.
  • the member to be treated is formed with a plurality of films without using an adhesive, there is no possibility that the adhesive component is eluted into the contents, and the contents It can be preferably applied to the case where the contents are food or pharmaceuticals. Furthermore, since the members to be treated are joined together by heating and pressing, the members to be treated can be integrated by simple means and can be preferably applied to a liquid container or the like, and the resin film is heated evenly. Separation is unlikely to occur on the joint surface, and it can be applied to fluid manifolds, etc., and has high industrial applicability.

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Treatments Of Macromolecular Shaped Articles (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
  • Lining Or Joining Of Plastics Or The Like (AREA)

Abstract

L'invention porte sur un procédé de modification de caractéristiques de surface dans une zone importante de divers matériaux en temps réel à l'aide d'un micro-plasma à pression atmosphérique. Un élément devant être traité est modifié en surface par irradiation de la surface de l'élément devant être traité avec un micro-plasma à pression atmosphérique qui est généré entre une pluralité d'électrodes de micro-plasma de 780 V à 1,9 kV à la pression atmosphérique en temps réel, sans utilisation d'une chambre sous vide. L'invention porte également sur un procédé de liaison utilisant le micro-plasma, qui est caractérisé en ce que les surfaces modifiées des éléments devant être traités sont liées ensemble en étant chauffées et pressées sans l'utilisation d'un adhésif.
PCT/JP2009/065986 2008-11-22 2009-09-08 Procédé de modification de surface utilisant un micro-plasma et procédé de liaison utilisant un micro-plasma Ceased WO2010058648A1 (fr)

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JP2010539182A JPWO2010058648A1 (ja) 2008-11-22 2009-09-08 マイクロプラズマを用いた表面改質処理方法及び接合方法

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012069448A (ja) * 2010-09-27 2012-04-05 Ngk Insulators Ltd プラズマ処理装置
WO2012173229A1 (fr) * 2011-06-16 2012-12-20 京セラ株式会社 Générateur de plasma et dispositif de génération de plasma
JP2016056363A (ja) * 2014-09-05 2016-04-21 国立大学法人大阪大学 表面改質成型体の製造方法、及び該表面改質成型体を用いた複合体の製造方法
JP2018087266A (ja) * 2016-11-28 2018-06-07 国立大学法人静岡大学 被処理体を修飾する方法及び被処理体を修飾する装置

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JPS6096445A (ja) * 1984-03-21 1985-05-30 Idemitsu Petrochem Co Ltd 樹脂積層体の製造方法
JPH05202208A (ja) * 1991-08-20 1993-08-10 Bridgestone Corp 加硫ゴムの表面処理方法
JPH0770335A (ja) * 1993-09-01 1995-03-14 Mitsui Toatsu Chem Inc 熱可塑性ポリイミド接着法およびその装置
JP2006302624A (ja) * 2005-04-19 2006-11-02 Matsushita Electric Works Ltd プラズマ処理装置及びプラズマ処理方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6096445A (ja) * 1984-03-21 1985-05-30 Idemitsu Petrochem Co Ltd 樹脂積層体の製造方法
JPH05202208A (ja) * 1991-08-20 1993-08-10 Bridgestone Corp 加硫ゴムの表面処理方法
JPH0770335A (ja) * 1993-09-01 1995-03-14 Mitsui Toatsu Chem Inc 熱可塑性ポリイミド接着法およびその装置
JP2006302624A (ja) * 2005-04-19 2006-11-02 Matsushita Electric Works Ltd プラズマ処理装置及びプラズマ処理方法

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012069448A (ja) * 2010-09-27 2012-04-05 Ngk Insulators Ltd プラズマ処理装置
WO2012173229A1 (fr) * 2011-06-16 2012-12-20 京セラ株式会社 Générateur de plasma et dispositif de génération de plasma
JPWO2012173229A1 (ja) * 2011-06-16 2015-02-23 京セラ株式会社 プラズマ発生体及びプラズマ発生装置
US9386678B2 (en) 2011-06-16 2016-07-05 Kyocera Corporation Plasma generator and plasma generating device
JP2016056363A (ja) * 2014-09-05 2016-04-21 国立大学法人大阪大学 表面改質成型体の製造方法、及び該表面改質成型体を用いた複合体の製造方法
JP2018087266A (ja) * 2016-11-28 2018-06-07 国立大学法人静岡大学 被処理体を修飾する方法及び被処理体を修飾する装置

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