JP5098181B2 - Application method - Google Patents
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- JP5098181B2 JP5098181B2 JP2006024222A JP2006024222A JP5098181B2 JP 5098181 B2 JP5098181 B2 JP 5098181B2 JP 2006024222 A JP2006024222 A JP 2006024222A JP 2006024222 A JP2006024222 A JP 2006024222A JP 5098181 B2 JP5098181 B2 JP 5098181B2
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本発明は、塗布方法に関するものであり、特に写真感光乳化剤、磁性材料液、反射防止性能等の機能を発現する光学薄膜用の塗布液などを、プラスチックフィルムや紙、金属箔等の可撓性支持体(以下、基材と称する)に塗布して、高機能を発現するシート状のものを製造するための塗布方法に関する。 The present invention relates to a coating method, in particular, a photographic photosensitive emulsifier, a magnetic material solution, a coating solution for an optical thin film that exhibits functions such as antireflection performance, and the like, such as plastic film, paper, and metal foil. The present invention relates to a coating method for producing a sheet-like material which is applied to a support (hereinafter referred to as a base material) and exhibits high functionality.
高機能を発現するシート状のものを製造するプロセスとして蒸着などのドライプロセスと塗布などのウェットプロセスの二つに分けられる。そのウェットプロセスにおいて近年ダイヘッドを用いたいわゆる「前計量タイプ」の塗布方式の利用が進んでいる。そのダイヘッドを用いる塗布方式の中でエクストルージョン方式においては、走行する基材に直接ダイヘッドを押し付けて塗布する方法と、バックアップロールに巻きつけて搬送される基材にダイヘッドの先端を近接させて塗布する方法がある。 There are two types of processes for producing sheet-like products that exhibit high functionality: dry processes such as vapor deposition and wet processes such as coating. In recent years, the so-called “pre-weighing type” coating method using a die head has been used in the wet process. Among the coating methods that use the die head, in the extrusion method, the die head is pressed directly onto the traveling substrate and applied, and the tip of the die head is applied close to the substrate that is wound around the backup roll and conveyed. There is a way to do it.
このダイヘッドを用いた塗布方法で生産における得率に大きく影響する部分として「塗り始め」の問題がある。塗布液が走行する基材に架橋してから定常の塗布状態(製品として認められる塗布状態)になるまでの間に製品として認められない部分が発生する問題のことで、この距離をなるべく短くすることがそのまま得率の向上に寄与する。そこで様々な手段がこれまで検討されてきた。
特にダイヘッドを使用して高速化を目的とする場合はロスが多くなるために問題が深刻化する。
There is a problem of “beginning of coating” as a part that greatly affects the yield in production by the coating method using this die head. This is a problem in which a portion that is not recognized as a product occurs between the time when the coating solution is cross-linked to the substrate to be traveled and the state where the coating solution is in a steady coating state (the coating state that is recognized as a product). This contributes to the improvement of the yield. Therefore, various means have been studied so far.
In particular, when a die head is used for the purpose of speeding up, the problem becomes serious because loss increases.
特許文献1では、ダイヘッドを50〜300μm/sの速度でバックアップロールに近づけつつ、定常時よりも高めの減圧度で塗り始める方法が示されている。この方法では条件によっては目的通りの塗り始めが可能だが、減圧度の規定がないため、定常時より高めの減圧度を設定した場合であっても塗布液がうまく基材に塗りつかないことがある。 Patent Document 1 discloses a method in which a die head is brought close to a backup roll at a speed of 50 to 300 μm / s and starts to be applied at a higher degree of reduced pressure than in a normal state. In this method, depending on the conditions, it is possible to start coating as intended, but since there is no regulation of the degree of vacuum, the coating liquid may not be applied well to the substrate even when a higher degree of vacuum is set than in the normal state. is there.
更に特許文献2に挙げられる方法も条件によってはうまくいくこともあるのだが、定常の塗布位置が基盤表面から離れている場合など、塗布液がうまく基材に塗りつかないことがある。 Furthermore, although the method described in Patent Document 2 may be successful depending on conditions, the coating solution may not be applied well to the substrate when the steady coating position is away from the substrate surface.
以下に先行技術文献を示す。
そこで搬送される基材にダイヘッドを近接させて塗布する方法において、塗り始めから定常部までの距離を短くして得率を向上させる必要がある。 Therefore, in the method of applying the die head close to the substrate to be transported, it is necessary to improve the yield by shortening the distance from the start of coating to the steady portion.
請求項1に係る発明は、搬送される基材に、塗布液を塗出させながらダイヘッド先端を近接させる工程、基材に近接させたダイヘッド先端を基材から離す工程、基材とダイヘッド先端を一定の距離(定常の塗布位置)に保ちながら塗布する工程、を有し、且つ、減圧チャンバーにより減圧させながら塗布する塗布方法において、該ダイヘッド先端を基材に近接させる工程が、基材とダイヘッド先端の間隙距離60μm以下になるまで近接させ、前記ダイヘッド先端を基材に近接させる工程時及び基材に近接させたダイヘッド先端を基材から離す工程時にダイヘッドから塗出される塗布液の塗出量が、基材とダイヘッド先端を一定の距離(定常の塗布位置)に保ちながら塗布する工程時のダイヘッドから塗出される塗布液の塗出量より5〜50%高く、前記ダイヘッド先端を基材に近接させる工程及び基材に近接させたダイヘッド先端を基材から離す工程において、ダイヘッド先端を基材に近接させた後、0.5〜5秒近接させた状態を保持した後、基材に近接させたダイヘッド先端を基材から離すことを特徴とする塗布方法である。
The invention according to claim 1 includes a step of bringing the tip of the die head close to the substrate to be conveyed while coating the coating liquid, a step of separating the tip of the die head that has been brought close to the substrate from the substrate, and the tip of the substrate and the die head. A step of applying while maintaining a constant distance (steady application position), and applying the pressure while reducing the pressure in a reduced pressure chamber. The amount of coating solution applied from the die head during the step of bringing the tip of the die head close to the substrate and the step of bringing the tip of the die head close to the substrate and the step of separating the tip of the die head close to the substrate away from the substrate. However, it is 5-50 from the coating amount of the coating liquid coated from the die head during the coating process while keeping the substrate and the tip of the die head at a constant distance (steady coating position). In the step of bringing the die head tip close to the base material and the step of separating the die head tip close to the base material from the base material, the die head tip is brought close to the base material and then brought close to the base material for 0.5 to 5 seconds. And holding the tip of the die head close to the base material away from the base material .
請求項2にかかる発明は、前記ダイヘッド先端を基材に近接させる工程時及び基材に近接させたダイヘッド先端を基材から離す工程時におけるチャンバー内の減圧度が、基材とダイヘッド先端を一定の距離(定常の塗布位置)に保ちながら塗布する工程時のチャンバー内の減圧度より0.1〜0.5kPa高いことを特徴とする請求項1記載の塗布方法である。 According to a second aspect of the present invention, the degree of pressure reduction in the chamber during the step of bringing the die head tip close to the substrate and the step of separating the die head tip brought close to the substrate from the substrate is constant between the substrate and the die head tip. 2. The coating method according to claim 1, which is 0.1 to 0.5 kPa higher than the degree of vacuum in the chamber during the coating process while maintaining the distance (steady coating position).
本発明の塗布方法では、基材への塗布液の架橋を確実に実行するタイミングと定常の塗布状態を作り出すタイミングとを別々に分けたことで、効率的に定常の塗布状態を作り出すことができる。また、基材への塗布液の架橋をより確実に実行することができる効果がある。 In the coating method of the present invention, the steady application state can be efficiently created by dividing the timing for reliably performing the crosslinking of the coating solution onto the substrate and the timing for creating the steady coating state separately. . Moreover, there exists an effect which can perform the bridge | crosslinking of the coating liquid to a base material more reliably.
ダイヘッドは、搬送される基材に対向する形で設置されており、ダイヘッドの形状や設置角度などには依存しない。そしてそのダイヘッドはいわゆる準備段階では基材に対して大きく離れた位置に待機しており、塗布開始とともに基材表面に近づける。本発明における塗布開始時とは、上記にあるようにダイヘッドを基材に近づける時をいっている。その近づける機構はサーボモーターや油圧などでLMガイド上を移動テーブルが精度良く動かされるものである。移動速度は1〜30mm/s程度が望ましいが、本発明はその速度に依存するものではない。 The die head is installed so as to face the substrate to be conveyed, and does not depend on the shape or the installation angle of the die head. In the so-called preparation stage, the die head stands by at a position far away from the substrate, and approaches the substrate surface as the application starts. The start of coating in the present invention refers to the time when the die head is brought close to the substrate as described above. The approaching mechanism is such that the moving table is moved on the LM guide with high accuracy by a servo motor or hydraulic pressure. The moving speed is preferably about 1 to 30 mm / s, but the present invention does not depend on the speed.
図1に理想的な塗り始めのシーケンスの例を示した。 FIG. 1 shows an example of an ideal coating start sequence.
最初に60μm以下にまで基材表面とダイヘッド先端との間隙距離L1を近づける。このときダイヘッドから塗布液は塗出させた状態になっている。この距離が大きすぎるとこの後の架橋がうまくいかないし、小さすぎると基材表面とダイヘッド先端が擦れることでゴミを発生させたりする可能性がある。 First, the gap distance L1 between the substrate surface and the tip of the die head is reduced to 60 μm or less. At this time, the coating liquid is applied from the die head. If this distance is too large, subsequent crosslinking will not be successful, and if it is too small, dust may be generated by rubbing the substrate surface and the tip of the die head.
減圧チャンバーをダイヘッドの基材流れ方向に対して上流側に設置し、塗布液が基材と接触する瞬間に上流側が減圧である必要がある。減圧にするためには減圧チャンバー(図示しない)内の空気をブロアで吸いだす。そのため予めこの減圧用のブロアは運転しながらダイヘッドを移動させる。このときのブロアの回転数は通常は定常時の値と一致させるが、一旦間隙を小さくするときに架橋がしにくいときもあるために、より高めの回転数にして減圧度を上げることが好ましい。つまり、ダイヘッド先端を近接させた時の減圧度P2を定常の塗布状態にある減圧度P1よりも高めに設定することが好ましい。その程度は減圧度にして0.1〜0.5kPa高めが望ましい。あまりこの値が小さいと効果がなくなるし、大きすぎると減圧に引き込まれてうまく液架橋が出来ない。 It is necessary to install a decompression chamber on the upstream side with respect to the substrate flow direction of the die head and to decompress the upstream side at the moment when the coating solution comes into contact with the substrate. In order to reduce the pressure, air in a vacuum chamber (not shown) is sucked out by a blower. Therefore, the die head is moved while operating the pressure reducing blower in advance. The rotational speed of the blower at this time is usually matched with the steady-state value, but it may be difficult to bridge once the gap is reduced. Therefore, it is preferable to increase the degree of pressure reduction at a higher rotational speed. . That is, it is preferable to set the pressure reduction degree P2 when the die head tips are close to each other to be higher than the pressure reduction degree P1 in the steady application state. The degree is preferably 0.1 to 0.5 kPa higher than the degree of decompression. If this value is too small, the effect will be lost, and if it is too large, it will be drawn into reduced pressure and liquid crosslinking will not be possible.
またダイヘッド先端を近接させた時の塗布液の塗出量Q2を定常の塗布状態にある塗布液の塗出量Q1よりも高めに設定してもよい。塗出量を高めに設定することは減圧度を高めにすることと両方実施しても良いし、塗出量だけ高めても問題ない。更にそのときの塗出量Q2は定常の塗布状態にある塗出量Q1より5〜50%高いことが望ましい。あまりこの値が小さいと効果がなく、大きすぎると確実な架橋に支障はないが、無駄に塗布液を流すことになり好ましくない。
ここで、図1の減圧度及び塗出量のグラフにおいて実線が二本引いてあるのは、ダイヘッド先端を基材に近接させる工程時及び基材に近接させたダイヘッド先端を基材から離す工程時におけるチャンバー内の減圧度及び塗出量と、基材とダイヘッド先端を一定の距離(定常の塗布位置)に保ちながら塗布する工程時のチャンバー内の減圧度及び塗出量とが変化することなく、理想的な塗布膜を形成することができる場合があるためである。
Further, the coating amount Q2 of the coating liquid when the tip of the die head is brought close may be set higher than the coating amount Q1 of the coating liquid in a steady coating state. Setting the coating amount to a higher value may be performed both for increasing the degree of decompression, or increasing only the coating amount. Furthermore, it is desirable that the coating amount Q2 at that time is 5 to 50% higher than the coating amount Q1 in a steady coating state. If this value is too small, there is no effect, and if it is too large, there is no hindrance to reliable crosslinking, but the coating solution is unnecessarily flown, which is not preferable.
Here, two solid lines are drawn in the graph of the degree of decompression and the coating amount in FIG. 1 when the die head tip is brought close to the substrate and the die head tip brought close to the substrate is separated from the substrate. The degree of decompression and the amount of coating in the chamber at the time, and the degree of decompression and the amount of coating in the chamber during the coating process while maintaining the substrate and the tip of the die head at a constant distance (steady coating position) must change. This is because an ideal coating film may be formed.
液架橋した後、ダイヘッド先端と基材表面との間隙距離を定常の塗布位置L2にまで広げる。このとき、ダイヘッド先端と基材表面との間隙距離が離れる変化と連動して、減圧度と塗出量を定常の塗布状態に変化させる。この動かすタイミングt2はダイヘッドの先端が基材表面に近接した時点t1から0.5〜5秒以内が望ましい。この時間があまり短すぎると確実な基材への液架橋が難しくなることもあり、長すぎると得率という観点で問題になる。 After the liquid crosslinking, the gap distance between the tip of the die head and the substrate surface is extended to the steady application position L2. At this time, the degree of reduced pressure and the coating amount are changed to a steady application state in conjunction with the change in the gap distance between the tip of the die head and the substrate surface. The moving timing t2 is preferably within 0.5 to 5 seconds from the time t1 when the tip of the die head approaches the substrate surface. If this time is too short, reliable liquid crosslinking to the substrate may be difficult, and if it is too long, there is a problem in terms of yield.
以上の動きをより正確に実行するためにはシーケンスを使用してダイヘッドの動きとそのときの減圧用のブロアの運転状況及びダイヘッドから塗出される塗布液の塗出量とを連動制御することが好ましい。 In order to execute the above movement more accurately, a sequence is used to control the movement of the die head, the operation status of the decompression blower at that time, and the coating amount of the coating liquid dispensed from the die head. preferable.
本発明に用いられる塗布液としては、酢酸メチル、酢酸エチル、酢酸ブチル、酢酸プロピル、メチルエチルケトン、メチルイソブチルケトン、アセトン、メタノール、エタノール、プロパノール、イソプロピルアルコール、エチレングリコール、エチレングリコールモノメチルエーテル、エチレングリコールモノメチルエーテルアセテート、プロピレングリコールモノメチルエーテル、プロピレングリコールモノメチルエーテルアセテート、トルエン、ジオキソラン、シクロヘキサノール、シクロヘキサノン、シクロヘキサンや水を希釈溶媒とした塗布液が考えられるが、これらに限定されるものではない。また、その塗布液の物性に効果は依存しない。塗布される湿潤膜厚にも依存性はないが、湿潤膜厚20μm以下の薄膜塗布により効果的である。 Examples of the coating solution used in the present invention include methyl acetate, ethyl acetate, butyl acetate, propyl acetate, methyl ethyl ketone, methyl isobutyl ketone, acetone, methanol, ethanol, propanol, isopropyl alcohol, ethylene glycol, ethylene glycol monomethyl ether, ethylene glycol monomethyl. A coating solution using ether acetate, propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, toluene, dioxolane, cyclohexanol, cyclohexanone, cyclohexane or water as a diluting solvent can be considered, but is not limited thereto. The effect does not depend on the physical properties of the coating solution. Although there is no dependence on the wet film thickness to be applied, it is more effective to apply a thin film having a wet film thickness of 20 μm or less.
幅650mmのポリエチレンテレフタレート基材を使用し、幅640mmのエクストルージョン型のダイヘッドを用いてメチルエチルケトン(MEK)と酢酸メチルを希釈溶剤とする50wt%のアクリル系のUV硬化樹脂塗布液を湿潤膜厚10μmとなるように50m/minの速度で塗布した。塗布液の粘度は4mPasで表面張力が25mN/mである。
定常の塗布位置にあるダイヘッド先端と基材表面との間隙L2は75μm、減圧度P1は1.5KPa、塗出量Q1は320cc/minである。
Using a polyethylene terephthalate substrate with a width of 650 mm, and using an extrusion type die head with a width of 640 mm, a 50 wt% acrylic UV curable resin coating solution containing methyl ethyl ketone (MEK) and methyl acetate as a diluent solvent has a wet film thickness of 10 μm. It was applied at a speed of 50 m / min. The coating solution has a viscosity of 4 mPas and a surface tension of 25 mN / m.
The gap L2 between the tip of the die head at the steady application position and the substrate surface is 75 μm, the degree of vacuum P1 is 1.5 KPa, and the coating amount Q1 is 320 cc / min.
ここで、ダイヘッドの先端が基材表面に近接した時のダイヘッド先端と基材との間隙L1を60μm、減圧度P2を1.6KPa、塗出量Q2を340cc/min、ダイヘッドの先端が基材表面に近接している時間t2−t1を0.5秒とし、実施例1のサンプルを得た。 Here, when the tip of the die head is close to the substrate surface, the gap L1 between the tip of the die head and the substrate is 60 μm, the degree of vacuum P2 is 1.6 KPa, the coating amount Q2 is 340 cc / min, and the tip of the die head is the substrate The sample of Example 1 was obtained by setting the time t2-t1 close to the surface to 0.5 seconds.
実施例1と同じ条件の下、P2を1.5KPaとし、実施例2のサンプルを得た。 Under the same conditions as in Example 1, P2 was set to 1.5 KPa, and the sample of Example 2 was obtained.
実施例1と同じ条件の下、Q2を320cc/minとし、実施例3のサンプルを得た。 Under the same conditions as in Example 1, Q2 was set to 320 cc / min, and the sample of Example 3 was obtained.
実施例1と同じ条件の下、P2を1.5KPa、Q2を320cc/minとし、実施例4のサンプルを得た。 Under the same conditions as in Example 1, P2 was set to 1.5 KPa, Q2 was set to 320 cc / min, and the sample of Example 4 was obtained.
<比較例1>
実施例1と同じ条件の下、t2−t1を0秒とし、比較例1のサンプルを得た。
<Comparative Example 1>
Under the same conditions as in Example 1, t2-t1 was set to 0 second to obtain a sample of Comparative Example 1.
<比較例2>
実施例1と同じ条件の下、L1を75μm、減圧度P2を1.5KPa、液流量Q2を320cc/minとし、比較例2のサンプルを得た。
<Comparative example 2>
Under the same conditions as in Example 1, L1 was 75 μm, the degree of vacuum P2 was 1.5 KPa, the liquid flow rate Q2 was 320 cc / min, and a sample of Comparative Example 2 was obtained.
<比較例3>
実施例1と同じ条件の下、L1を90μm、減圧度P2を1.5KPa、液流量Q2を320cc/minとし、比較例3のサンプルを得た。
<Comparative Example 3>
Under the same conditions as in Example 1, L1 was 90 μm, the degree of vacuum P2 was 1.5 KPa, the liquid flow rate Q2 was 320 cc / min, and a sample of Comparative Example 3 was obtained.
以上のようにパラメーターを変化させて塗布状態を確認した。結果を表1に示す。ここでは、n=10で塗布面が幅方向に問題なく塗布できた回数を記録した。 As described above, the coating state was confirmed by changing the parameters. The results are shown in Table 1. Here, the number of times that the coating surface was successfully applied in the width direction when n = 10 was recorded.
以上の結果より、ダイヘッド先端と基材表面との間隙を狭くすることで塗り始めの状態がよくなり、塗布開始時及び基材に近接させたダイヘッド先端が定常の塗布位置に離れ始める時までの塗出量を増やしたり、減圧度を増やすことで更にその確率が上がることがわかる。また、ダイヘッド先端を基材に近接させた後、0.5秒以上近接した状態を保持することでその確率が高まることがわかる。
From the above results, the state of the start of coating is improved by narrowing the gap between the tip of the die head and the surface of the substrate, and until the start of coating and the tip of the die head that is close to the substrate starts to move away to the steady coating position. It can be seen that the probability is further increased by increasing the coating amount or increasing the degree of decompression. It can also be seen that the probability is increased by keeping the die head tip close to the substrate and then keeping the state close to 0.5 seconds or more.
本発明は、塗布方法に関するものであり、特に写真感光乳化剤、磁性材料液、反射防止性能等の機能を発現する光学薄膜用の塗布液などを、プラスチックフィルムや紙、金属箔等の基材に塗布して、高機能を発現するシート状のものを製造する場合に有効である。 The present invention relates to a coating method, and in particular, a photographic photosensitive emulsifier, a magnetic material solution, a coating solution for an optical thin film that exhibits functions such as antireflection performance, and the like on a substrate such as a plastic film, paper, or metal foil. It is effective when applied to produce a sheet-like material that exhibits high functionality.
L1 ダイヘッドの先端が基材表面に近接した時のダイヘッド先端と基材表面との間隙距離
L2 定常の塗布状態でのダイヘッド先端と基材表面の間隙距離
P1 定常の塗布状態での減圧度
P2 塗布開始時から基材に近接させたダイヘッド先端が定常の塗布位置に離れ始めるまでの減圧度
Q1 定常の塗布状態での塗出量
Q2 塗布開始時から基材に近接させたダイヘッド先端が定常の塗布位置に離れ始めるまでの塗出量
t1 ダイヘッド先端が基材表面に近接した時間
t2 ダイヘッド先端が定常の塗布位置に離れ始める時間
L1 Gap distance L2 between the die head tip and the substrate surface when the tip of the die head comes close to the substrate surface L2 Gap distance P1 between the die head tip and the substrate surface in a steady coating state P1 Decompression degree P2 in a steady coating state Degree of decompression Q1 until the tip of the die head close to the substrate starts to move to the steady coating position Q1 Coating amount Q2 in the steady coating state Steady coating of the die head tip close to the substrate from the start of coating Coating amount t1 until it starts to move to the position t1 Time when the tip of the die head comes close to the surface of the substrate t2 Time when the tip of the die head starts to move away from the steady coating position
Claims (2)
基材に近接させたダイヘッド先端を基材から離す工程、
基材とダイヘッド先端を一定の距離(定常の塗布位置)に保ちながら塗布する工程、
を有し、
且つ、減圧チャンバーにより減圧させながら塗布する塗布方法において、
該ダイヘッド先端を基材に近接させる工程が、基材とダイヘッド先端の間隙距離60μm以下になるまで近接させ、
前記ダイヘッド先端を基材に近接させる工程時及び基材に近接させたダイヘッド先端を基材から離す工程時にダイヘッドから塗出される塗布液の塗出量が、基材とダイヘッド先端を一定の距離(定常の塗布位置)に保ちながら塗布する工程時のダイヘッドから塗出される塗布液の塗出量より5〜50%高く、
前記ダイヘッド先端を基材に近接させる工程及び基材に近接させたダイヘッド先端を基材から離す工程において、
ダイヘッド先端を基材に近接させた後、0.5〜5秒近接させた状態を保持した後、基材に近接させたダイヘッド先端を基材から離すことを特徴とする塗布方法。 A step of bringing the tip of the die head close to the substrate to be conveyed while coating the coating liquid;
A step of separating the tip of the die head close to the substrate from the substrate;
Applying while keeping the substrate and die head tip at a fixed distance (steady application position),
Have
And in the coating method of applying while reducing the pressure in the vacuum chamber,
The step of bringing the tip of the die head close to the substrate is brought close to the gap distance of 60 μm or less between the substrate and the tip of the die head,
The amount of coating liquid applied from the die head during the step of bringing the tip of the die head close to the substrate and the step of separating the tip of the die head close to the substrate from the substrate is a constant distance between the substrate and the tip of the die head ( 5 to 50% higher than the application amount of the application liquid applied from the die head during the application process while maintaining the constant application position)
In the step of bringing the die head tip close to the substrate and the step of separating the die head tip brought close to the substrate from the substrate,
An application method comprising: bringing a die head tip close to a substrate, holding the state of being brought close to 0.5 to 5 seconds, and then separating the die head tip brought close to the substrate from the substrate.
The degree of pressure reduction in the chamber during the step of bringing the die head tip close to the base material and the step of separating the die head tip close to the base material from the base material is a constant distance between the base material and the die head tip (steady coating position) The coating method according to claim 1, wherein the coating pressure is higher by 0.1 to 0.5 kPa than the degree of vacuum in the chamber during the coating step.
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