JP3832268B2 - Photoresist liquid product manufacturing method - Google Patents
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Description
【０００１】
【発明の属する技術分野】
本発明はフォトレジスト液製品の製造方法に関し、詳しくは、紫外線、遠紫外線、電子線、Ｘ線等の放射線によって作用するリソグラフィに適したフォトレジスト液製品を製造する方法に関するものである。
【０００２】
【従来の技術】
フォトレジスト液製品は、従来、フォトレジストを構成する各成分を混合する混合槽と、複数のバルブと、フッ素系樹脂製及びポリオレフィン製のフィルターから選ばれる１種以上のフィルターが格納されたフィルターハウジングと、上記混合槽、バルブ及びフィルターハウジングを接続する配管とからなる装置を用いて、フッ素系樹脂製及びポリオレフィン製のフィルターから選ばれる１種以上のフィルターにより、原料フォトレジスト液を濾過して製造されていた。
【０００３】
【発明が解決しようとする課題】
しかしながら、上記フィルターは繰り返し濾過操作に使用すると、フィルターに捕捉された微粒子により目詰まりしてしまい、事実上使い捨てになるため、従来の製造方法は、結果的にコストがかさむものであった。
【０００４】
【課題を解決するための手段】
本発明者は、コストがかさまないフォトレジスト液製品の製造方法を提供すべく鋭意検討した結果、上記混合槽内で調製された原料フォトレジスト液の濾過に使用されたフッ素系樹脂製及びポリオレフィン製のフィルターから選ばれる１種以上のフィルターが格納されたフィルターハウジングを、混合槽からフィルターハウジング入口部までの装置内を洗浄して得た少なくともＮ−メチルピロリドンを含む洗浄液により、濾過時の方向とは逆向きに洗浄し、この逆洗浄されたフィルターを用いて原料フォトレジスト液を濾過すると、上記課題が解決されることを見出し、本発明を完成するに至った。
【０００５】
即ち、本発明は、フォトレジストを構成する感光剤成分、樹脂成分及び溶媒成分を混合する混合槽と、複数のバルブと、フッ素系樹脂製及びポリオレフィン製のフィルターから選ばれる１種以上のフィルターが格納されたフィルターハウジングと、上記混合槽、バルブ及びフィルターハウジングを接続する配管とからなる装置を用い、下記（ａ）〜（ｄ）の工程を行うことを特徴とするフォトレジスト液製品の製造方法を提供するものである。
（ａ）上記混合槽内で調製された原料フォトレジスト液を、フィルターハウジング内で濾過する工程、
（ｂ）次いで、混合槽からフィルターハウジング入口部までの装置内を、Ｎ−メチルピロリドンと混和する溶媒成分を含んでいてもよい、Ｎ−メチルピロリドンを用いて洗浄する工程、
（ｃ）工程（ａ）で得た１種以上の湿潤フィルターを、工程（ｂ）で得た洗浄液を用いて、濾過時の方向とは逆向きに洗浄する工程、
（ｄ）工程（ｃ）で逆洗浄されたフィルターにより、工程（ａ）の原料フォトレジスト液と同種又は異種の原料フォトレジスト液を濾過する工程：
但し、工程（ｄ）で濾過する原料フォトレジスト液が工程（ａ）の原料フォトレジスト液と異種である場合は、両者のフォトレジスト液を構成する溶媒は同一である。
【０００６】
【発明の実施の形態】
以下、本発明を詳細に説明する。
本発明において用いられる原料フォトレジスト液は、上記リソグラフィに適用できるものであればよいが、好ましくは、上記フォトレジスト液中の感光剤成分が、Ｎ−メチルピロリドンの希薄濃度溶液中において、容易に分解するものを挙げることができる。このような感光剤成分としては、例えば、ｏ−ベンゾキノンジアジドスルホン酸エステル、ｏ−ベンゾキノンジアジドスルホン酸アミド、ｏ−ナフトキノンジアジドスルホン酸エステルやｏ−ナフトキノンジアジドスルホン酸アミドのようなキノンジアジドスルホン酸エステル及びキノンジアジドスルホン酸アミド等が挙げられる。
【０００７】
フォトレジスト液を構成する溶媒成分としては、Ｎ−メチルピロリドンと混和するものが好ましい。このような有機溶媒としては、プロピレングリコールモノメチルエーテルアセテート、アセトン、メチルイソブチルケトン、２−ヘプタノン、シクロヘキサノン、γ−ブチロラクトン、乳酸エチル、酢酸ブチル、酢酸アミル、ピルビン酸エチル、ジエチレングリコールジメチルエーテル、メチルセロソルブアセテート及びエチルセロソルブアセテート等が例示される。
工程（ａ）及び（ｄ）の原料フォトレジスト液中の樹脂成分としては、アルカリ可溶性樹脂が好ましい。アルカリ可溶性樹脂としては、例えば、ポジ型フォトレジストに用いられるノボラック樹脂が好ましい。
【０００８】
本発明は、上記混合槽内で調製された原料フォトレジスト液の濾過に使用されたフッ素系樹脂製及びポリオレフィン製のフィルターから選ばれる１種以上のフィルターを、混合槽からフィルターハウジング入口部までの装置内を洗浄して得た、上記フォトレジストを構成する溶媒成分と同一もしくは異なる溶媒成分を含んでいてもよい、Ｎ−メチルピロリドンの洗浄液により、濾過時の方向とは逆向きに洗浄し、この逆洗浄されたフィルターを用いて原料フォトレジスト液を濾過することを特徴とするものであり、原料フォトレジスト液を一旦フッ素系樹脂製のフィルターに通過させ、その後、ポリオレフィン製のフィルターに通過させる方法が好ましい。
本発明において用いられるフッ素系樹脂製フィルターとしては、ポリテトラフルオロエチレン製のものが好ましい。又、ポリオレフィン製フィルターとしては、ポリエチレン製のものが好ましい。
逆洗浄後に再使用するフィルターとしては、ポリエチレン製のフィルターが好ましい。
フィルターの逆洗浄の際には、原料フォトレジスト液に含まれる感光剤成分が、Ｎ−メチルピロリドン溶液中において、1〜200ｐｐｍの範囲の希薄濃度になる
ことが好ましい。例えば、ｏ−ベンゾキノンジアジドスルホン酸エステル、ｏ−ベンゾキノンジアジドスルホン酸アミド、ｏ−ナフトキノンジアジドスルホン酸エステルやｏ−ナフトキノンジアジドスルホン酸アミド等のポジ型フォトレジストに用いられる感光剤成分は、比較的、フォトレジスト液中の微粒子数の増加原因となりやすいが、フィルターに残存している感光剤成分が上記濃度範囲でＮ−メチルピロリドンにより分解されやすいので、効率的な逆洗浄を行うことが可能になる。
【０００９】
本発明で用いられるポリテトラフルオロエチレン製のフィルターとしては、例えば、ＡＢＤ１ＵＦＤ３Ｅ［日本ポール（株）製］、ＡＢＤ１ＵＦＴ３ＥＮ［日本ポール（株）製］等が挙げられる。孔径は、通常0.01〜１μｍ程度のものが使用される。又、ポリエチレン製のフィルターとしては、例えば、ＳＨ４Ｍ２２８Ｊ３［日本ミリポア（株）製］、ＣＳ０９ＸＦＥ［三菱化成（株）製］、ＣＳ２０ＸＦＥ［三菱化成（株）製］等が挙げられる。孔径は、通常0.01〜0.2μｍ程度のものが使用される。
【００１０】
【実施例】
以下、実施例等により、本発明を更に詳細に説明する。
【００１１】
参考例１
図３に記載の装置［配管における太線及び矢印は、液の流れ方向を示す］を用いて、原料フォトレジスト液の濾過を行い、ＰＦＩ−３２Ａ６［アルカリ可溶性ノボラック樹脂、キノンジアジドスルホン酸エステル系感光剤及び２−ヘプタノンからなる住友化学工業（株）製のポジ型フォトレジスト液製品］を得た。なお、図３記載の釜（１）内には、アルカリ可溶性ノボラック樹脂、キノンジアジドスルホン酸エステル系感光剤及び２−ヘプタノン等を混合することにより調製された上記ＰＦＩ−３２Ａ６（原料フォトレジスト液）の残液が溜まっている。図３のフィルターハウジング（３）には、フィルターとして、ポリエチレン製のＳＨ４Ｍ２２８Ｊ３［孔径０．２μｍ、日本ミリポア（株）製］が格納されており、上記ポリエチレン製フィルターは、原料フォトレジスト液を一回濾過することにより、湿潤されている。なお、フィルターハウジング（２）は、溶媒由来の微粒子のカットを主目的として設けている。
【００１２】
次いで、バルブ（５）を閉じ、且つ、バルブ（５）の右側下方に位置するバルブ（１１）を開けた状態で、上記原料フォトレジストの残液が溜まった釜（１）から、フィルターハウジング（２）を経由して、フィルターハウジング（３）の下方に位置するバルブ（５）までの流路を、２−ヘプタノン、Ｎ−メチルピロリドン及び２−ヘプタノンを用いて、この順に洗浄した。
２−ヘプタノン１４．１ｋｇによる粗洗浄後、洗浄液を回収した。これを回収２−ヘプタノンとした。
次に、Ｎ−メチルピロリドンをそれぞれ５．４ｋｇ及び７ｋｇ使用して２回洗浄（以下、ＮＭＰ洗浄という）し、洗浄液を回収した。これらを合わせて回収ＮＭＰとした。
最後は、２−ヘプタノンによる置換洗浄を７回行い、それぞれ順に、２−ヘプタノンを５ｋｇ、６．２ｋｇ、６ｋｇ、７．２ｋｇ、６ｋｇ、８ｋｇ及び７ｋｇ使用した。６回目及び７回目の洗浄液を合わせて回収２−ヘプタノンとした。
粗洗浄後に得られた回収２−ヘプタノン中の感光剤濃度は１．５ｐｐｍであった。又、回収ＮＭＰは感光剤が検出されなかった。そして、１回目の置換洗浄後に得られた液中のＮＭＰ濃度は２８０７ｐｐｍであり、６回目の置換洗浄後に得られた液中のＮＭＰ濃度は５９ｐｐｍであり、７回目の置換洗浄後に得られた液中のＮＭＰ濃度は２９ｐｐｍであった。なお、フィルターハウジング（２）は、溶媒由来の微粒子のカットを主目的として設けている。
【００１３】
実施例１
図１に記載の装置を使用し、参考例１の粗洗浄後に得た回収２−ヘプタノン、回収ＮＭＰ、及び、置換洗浄により得た回収２−ヘプタノンをこの順に用いて、フィルターハウジング（３）内に格納されたポリエチレン製のフィルター（前記参考例１において、原料フォトレジスト液の濾過に用いたＳＨ４Ｍ２２８Ｊ３）を逆洗浄した。具体的には、バルブ（７）、バルブ（８）、バルブ（９）、フィルターハウジング（３）及びバルブ（１０）の経路で上記の回収溶媒を通液し［太線及び矢印で示した流れ方向］、それぞれ順に、回収２−ヘプタノン洗浄液約１４ｋｇ、回収ＮＭＰ洗浄液約１２ｋｇ、及び、回収２−ヘプタノン洗浄液約１５ｋｇを得た。
上記の回収溶媒による逆洗浄後、前記回収溶媒洗浄液を蒸留して、それぞれ、蒸留２−ヘプタノン約１３ｋｇ、蒸留ＮＭＰ約１１ｋｇ及び蒸留２−ヘプタノン約１４ｋｇを得た。
【００１４】
次に、これらの蒸留溶媒のうち、ＮＭＰ約７ｋｇ及び２−ヘプタノン約２６ｋｇをこの順に用いて、バルブ（７）、バルブ（８）、バルブ（９）、フィルターハウジング（３）及びバルブ（１０）の経路で上記の蒸留溶媒を通液［太線及び矢印で示した流れ方向（図３を参照）］し、ポリエチレン製フィルター（ＳＨ４Ｍ２２８Ｊ３）を逆洗浄して、それぞれ、回収ＮＭＰ洗浄液約７ｋｇ及び回収２−ヘプタノン洗浄液約２６ｋｇを得た。
【００１５】
参考例２
ポリエチレン製のフィルターＳＨ４Ｍ２２８Ｊ３（購入直後の新品を２−ヘプタノンで湿潤させたもの）と、実施例１で得た逆洗浄後のポリエチレン製フィルターＳＨ４Ｍ２２８Ｊ３（以下、再使用品という）とを、図２記載のフィルターハウジング（３）内にそれぞれ別個に装着し、図２記載の装置を用いて以下に記すテストを行った。
【００１６】
＜粒子除去性能に影響するフィルター微細孔構造の損壊有無の確認試験＞
フィルターハウジング（３）の側部に設けたバルブ（５）から窒素ガスを導入し、バルブ（６）を調節することにより、上記装着したフィルターを一定時間加圧後、拡散通過ガス量を捕集して、フィルター微細孔構造の損壊有無を試験した。窒素圧１５０ｋＰａにおいても、再使用品の拡散通過ガス量は、新品フィルターの拡散通過ガス量以下であり、フィルターの微細孔構造の損壊がないことが確認された。
【００１７】
参考例３
実施例１で得たポリエチレン製フィルターＳＨ４Ｍ２２８Ｊ３（再使用品）を上記ＰＦＩ−３２Ａ６（フォトレジスト液製品）に浸漬し、前記ＰＦＩ−３２Ａ６製品（フィルターの浸漬はなし）を対照として、０．２μｍ径以上の微粒子数の変化を経時的に試験して、表１の結果を得た。
【００１８】
表１のとおり、室温以上の温度では、微粒子数の増加は認められなかった。このことから、実施例１で得た再使用ポリエチレン製フィルターは２−ヘプタノンに対する耐性に優れており、このフィルターをフォトレジスト液の濾過に使用しても、微粒子数増加の原因にならないことが判る。
【００２０】
実施例２
図３記載の装置［実施例１で得たポリエチレン製フィルター（再使用品）をフィルターハウジング（３）内に装着している。又、フィルターハウジング（２）は、原料レジストを構成する溶媒由来の微粒子のカットを主目的として設けている。尚、配管における太線及び矢印は、液の流れ方向を示す］を用い、参考例１で使用した原料フォトレジスト液を、窒素ガス加圧によるワンパス方式で濾過した結果、０．２μｍ径以上の微粒子数の少ないフォトレジスト製品が得られた。本例では窒素ガス加圧によるワンパス方式で濾過したが、ポンプを用いて循環方式で濾過しても、ワンパス方式と同様、微粒子数の少ないフォトレジスト製品が得られる。
【００２１】
【発明の効果】
本発明によれば、フォトレジスト製品を工業的有利に製造することができる。
【図面の簡単な説明】
【図１】実施例１で用いた装置
【図２】参考例２で用いた装置
【図３】参考例１で用いた装置
【符号の説明】
１・・釜、２・・フィルターハウジング、３・・フィルターハウジング、４・・逆洗浄入口部、５・・開閉用バルブ、６・・圧力調節用バルブ、７〜１１・・開閉用バルブ[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for producing a photoresist liquid product, and more particularly to a method for producing a photoresist liquid product suitable for lithography that acts by radiation such as ultraviolet rays, far ultraviolet rays, electron beams, and X-rays.
[0002]
[Prior art]
Conventionally, a photoresist liquid product is a filter housing in which at least one type of filter selected from a mixing tank for mixing components constituting a photoresist, a plurality of valves, and a filter made of fluororesin and polyolefin is stored. And using a device comprising the above-mentioned mixing tank, a valve and a pipe connecting the filter housing, the raw photoresist solution is filtered through one or more filters selected from fluororesin and polyolefin filters. It had been.
[0003]
[Problems to be solved by the invention]
However, when the filter is repeatedly used for filtration operations, the filter is clogged with fine particles trapped in the filter and becomes practically disposable. As a result, the conventional manufacturing method is costly.
[0004]
[Means for Solving the Problems]
As a result of earnest studies to provide a method for producing a photoresist liquid product that does not cost much, the present inventors have made a fluororesin and a polyolefin that have been used for filtering the raw photoresist liquid prepared in the mixing tank. Direction at the time of filtration with a cleaning liquid containing at least N-methylpyrrolidone obtained by cleaning the inside of the apparatus from the mixing tank to the inlet of the filter housing in the filter housing in which one or more types of filters selected from manufactured filters are stored When the raw photoresist solution was filtered using the back-washed filter, it was found that the above problems were solved, and the present invention was completed.
[0005]
That is, the present invention includes at least one filter selected from a mixing tank for mixing a photosensitive agent component, a resin component, and a solvent component constituting a photoresist, a plurality of valves, and a fluororesin and polyolefin filter. A method for producing a photoresist liquid product, characterized in that the following steps (a) to (d) are performed using an apparatus comprising a stored filter housing and a pipe connecting the mixing tank, the valve and the filter housing. Is to provide.
(A) filtering the raw material photoresist solution prepared in the mixing tank in a filter housing;
(B) Next, the step of cleaning the inside of the apparatus from the mixing tank to the filter housing inlet with N-methylpyrrolidone, which may contain a solvent component miscible with N-methylpyrrolidone ,
(C) a step of washing one or more wet filters obtained in step (a) using the washing liquid obtained in step (b) in a direction opposite to the direction during filtration;
(D) The step of filtering the same or different raw photoresist liquid as the raw photoresist liquid in the step (a) with the filter back-washed in the step (c):
However, when the raw material photoresist solution to be filtered in the step (d) is different from the raw material photoresist solution in the step (a), the solvents constituting the both photoresist solutions are the same.
[0006]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, the present invention will be described in detail.
The raw material photoresist solution used in the present invention may be any material that can be applied to the lithography. Preferably, the photosensitive agent component in the photoresist solution is easily dissolved in a dilute solution of N-methylpyrrolidone. The thing which decomposes | disassembles can be mentioned. Examples of such a photosensitizer component include o-benzoquinone diazide sulfonic acid ester, o-benzoquinone diazide sulfonic acid amide, o-naphthoquinone diazide sulfonic acid ester, and quinone diazide sulfonic acid ester such as o-naphthoquinone diazide sulfonic acid amide, and And quinonediazide sulfonic acid amide.
[0007]
As the solvent component constituting the photoresist solution, those miscible with N-methylpyrrolidone are preferable. Such organic solvents include propylene glycol monomethyl ether acetate, acetone, methyl isobutyl ketone, 2-heptanone, cyclohexanone, γ-butyrolactone, ethyl lactate, butyl acetate, amyl acetate, ethyl pyruvate, diethylene glycol dimethyl ether, methyl cellosolve acetate and Examples include ethyl cellosolve acetate.
As the resin component in the raw material photoresist solution in the steps (a) and (d), an alkali-soluble resin is preferable. As the alkali-soluble resin, for example, a novolac resin used for a positive photoresist is preferable.
[0008]
The present invention provides at least one type of filter selected from the fluororesin and polyolefin filters used for filtering the raw material photoresist solution prepared in the mixing tank from the mixing tank to the filter housing inlet. obtained by washing the inside of the apparatus may include a solvent component and a same or different solvent components constituting the upper Symbol photoresist, the cleaning liquid of N- methylpyrrolidone, and washed in the opposite direction to the direction of filtration The raw photoresist solution is filtered using this back-washed filter. The raw photoresist solution is once passed through a fluororesin filter and then passed through a polyolefin filter. The method of making it preferable is.
The fluororesin filter used in the present invention is preferably a polytetrafluoroethylene filter. The polyolefin filter is preferably a polyethylene filter.
As a filter to be reused after backwashing, a polyethylene filter is preferable.
In the backwashing of the filter, it is preferable that the photosensitive agent component contained in the raw photoresist solution has a dilute concentration in the range of 1 to 200 ppm in the N-methylpyrrolidone solution. For example, photosensitizer components used in positive photoresists such as o-benzoquinone diazide sulfonic acid ester, o-benzoquinone diazide sulfonic acid amide, o-naphthoquinone diazide sulfonic acid ester and o-naphthoquinone diazide sulfonic acid amide are relatively Although it tends to cause an increase in the number of fine particles in the photoresist solution, the photosensitizer component remaining on the filter is easily decomposed by N-methylpyrrolidone within the above concentration range, so that efficient back cleaning can be performed. .
[0009]
Examples of the filter made of polytetrafluoroethylene used in the present invention include ABD1UFD3E [manufactured by Nippon Pole Co., Ltd.], ABD1UFT3EN [manufactured by Nippon Pole Co., Ltd.], and the like. A pore diameter of about 0.01 to 1 μm is usually used. Examples of the polyethylene filter include SH4M228J3 [manufactured by Nippon Millipore Corporation], CS09XFE [manufactured by Mitsubishi Kasei Corporation], CS20XFE [manufactured by Mitsubishi Kasei Corporation], and the like. The pore diameter is usually about 0.01 to 0.2 μm.
[0010]
【Example】
Hereinafter, the present invention will be described in more detail with reference to examples and the like.
[0011]
Reference example 1
The raw photoresist solution is filtered using the apparatus shown in FIG. 3 [thick lines and arrows in the pipes indicate the flow direction of the liquid], and PFI-32A6 [alkali-soluble novolak resin, quinonediazide sulfonate ester photosensitizer] And a positive photoresist liquid product manufactured by Sumitomo Chemical Co., Ltd., comprising 2-heptanone]. In addition, in the pot (1) shown in FIG. 3, the PFI-32A6 (raw material photoresist solution) prepared by mixing an alkali-soluble novolak resin, a quinonediazide sulfonate ester photosensitizer, 2-heptanone, and the like. Residual liquid has accumulated. The filter housing (3) in FIG. 3 stores SH4M228J3 [pore size 0.2 μm, manufactured by Nippon Millipore Co., Ltd.] as a filter, and the polyethylene filter uses a raw photoresist solution once. Wet by filtering. The filter housing (2) is provided mainly for cutting fine particles derived from the solvent.
[0012]
Next, with the valve (5) closed and the valve (11) located below the right side of the valve (5) opened, the filter housing (1) The flow path through 2) to the valve (5) located below the filter housing (3) was washed in this order using 2-heptanone, N-methylpyrrolidone and 2-heptanone.
After rough washing with 14.1 kg of 2-heptanone, the washing liquid was recovered. This was designated as recovered 2-heptanone.
Next, N-methylpyrrolidone was washed twice using 5.4 kg and 7 kg, respectively (hereinafter referred to as NMP washing), and the washing liquid was recovered. These were combined to obtain recovered NMP.
Finally, substitution washing with 2-heptanone was performed 7 times, and 2-heptanone was used in order of 5 kg, 6.2 kg, 6 kg, 7.2 kg, 6 kg, 8 kg and 7 kg, respectively. The 6th and 7th washings were combined to obtain recovered 2-heptanone.
The concentration of the photosensitizer in the recovered 2-heptanone obtained after the rough washing was 1.5 ppm. Further, no photosensitizer was detected in the recovered NMP. The NMP concentration in the liquid obtained after the first substitution washing is 2807 ppm, the NMP concentration in the liquid obtained after the sixth substitution washing is 59 ppm, and the liquid obtained after the seventh substitution washing. The NMP concentration therein was 29 ppm. The filter housing (2) is provided mainly for cutting fine particles derived from the solvent.
[0013]
Example 1
Using the apparatus shown in FIG. 1, the recovered 2-heptanone, the recovered NMP, and the recovered 2-heptanone obtained by the substitution cleaning in Reference Example 1 were used in this order in the filter housing (3). The filter made of polyethylene (SH4M228J3 used for filtering the raw material photoresist solution in Reference Example 1) was back-washed. Specifically, the recovered solvent is passed through the path of the valve (7), the valve (8), the valve (9), the filter housing (3), and the valve (10) [flow direction indicated by thick lines and arrows. ] About 14 kg of recovered 2-heptanone cleaning liquid, about 12 kg of recovered NMP cleaning liquid, and about 15 kg of recovered 2-heptanone cleaning liquid were obtained in this order.
After backwashing with the recovered solvent, the recovered solvent cleaning solution was distilled to obtain about 13 kg of distilled 2-heptanone, about 11 kg of distilled NMP, and about 14 kg of distilled 2-heptanone, respectively.
[0014]
Next, among these distilled solvents, about 7 kg of NMP and about 26 kg of 2-heptanone are used in this order, and the valve (7), valve (8), valve (9), filter housing (3) and valve (10) are used. And the polyethylene filter (SH4M228J3) was back-washed by passing the above-mentioned distillation solvent through the above-mentioned route [flow direction indicated by bold lines and arrows (see FIG. 3)], and about 7 kg of recovered NMP cleaning solution and recovered 2 respectively. -About 26 kg of heptanone washing solution was obtained.
[0015]
Reference example 2
FIG. 2 shows a polyethylene filter SH4M228J3 (a new product immediately after purchase was wetted with 2-heptanone) and a polyethylene filter SH4M228J3 (hereinafter referred to as a reusable product) obtained in Example 1 after backwashing. Each of the filter housings (3) was mounted separately, and the following test was performed using the apparatus shown in FIG.
[0016]
<Confirmation test of filter micropore structure that affects particle removal performance>
Nitrogen gas is introduced from a valve (5) provided on the side of the filter housing (3), and the valve (6) is adjusted to pressurize the attached filter for a certain period of time, and then collect the amount of diffusion gas passing through Then, the presence or absence of breakage of the filter micropore structure was tested. Even at a nitrogen pressure of 150 kPa, it was confirmed that the amount of diffusion pass gas of the reused product was not more than the amount of diffusion pass gas of the new filter, and the fine pore structure of the filter was not damaged.
[0017]
Reference example 3
The polyethylene filter SH4M228J3 (reusable product) obtained in Example 1 was immersed in the PFI-32A6 (photoresist solution product), and the PFI-32A6 product (no filter was immersed) was used as a control. The change in the number of fine particles was tested over time, and the results in Table 1 were obtained.
[0018]
As shown in Table 1, no increase in the number of fine particles was observed at temperatures above room temperature. From this, it can be seen that the reused polyethylene filter obtained in Example 1 is excellent in resistance to 2-heptanone, and even if this filter is used for filtration of a photoresist solution, it does not cause an increase in the number of fine particles. .
[0020]
Example 2
The apparatus shown in FIG. 3 [The polyethylene filter (reused product) obtained in Example 1 is mounted in the filter housing (3). The filter housing (2) is provided mainly for cutting fine particles derived from the solvent constituting the raw material resist. In addition, as a result of filtering the raw material photoresist liquid used in Reference Example 1 by a one-pass method using nitrogen gas pressurization, fine particles having a diameter of 0.2 μm or more are used. A few photoresist products were obtained. In this example, filtration is performed by a one-pass method using nitrogen gas pressurization. However, even if filtration is performed by a circulation method using a pump, a photoresist product with a small number of fine particles can be obtained as in the one-pass method.
[0021]
【The invention's effect】
According to the present invention, a photoresist product can be produced industrially advantageously.
[Brief description of the drawings]
FIG. 1 shows the apparatus used in Example 1. FIG. 2 shows the apparatus used in Reference Example 2. FIG. 3 shows the apparatus used in Reference Example 1.
1 .... Kan, 2 .... Filter housing, 3 .... Filter housing, 4 .... Backwash inlet, 5 .... Open / close valve, 6 .... Pressure adjusting valve, 7-11 ... Open / close valve
Claims (9)
（ａ）上記混合槽内で調製された原料フォトレジスト液を、フィルターハウジング内で濾過する工程、
（ｂ）次いで、混合槽からフィルターハウジング入口部までの装置内を、Ｎ−メチルピロリドンと混和する溶媒成分を含んでいてもよい、Ｎ−メチルピロリドンを用いて洗浄する工程、
（ｃ）工程（ａ）で得た１種以上の湿潤フィルターを、工程（ｂ）で得た洗浄液を用いて、濾過時の方向とは逆向きに洗浄する工程、
（ｄ）工程（ｃ）で逆洗浄されたフィルターにより、工程（ａ）の原料フォトレジスト液と同種又は異種の原料フォトレジスト液を濾過する工程：
但し、工程（ｄ）で濾過する原料フォトレジスト液が工程（ａ）の原料フォトレジスト液と異種である場合は、両者のフォトレジスト液を構成する溶媒は同一である。A mixing tank for mixing a photosensitive agent component, a resin component, and a solvent component constituting the photoresist, a plurality of valves, and a filter housing in which one or more types of filters selected from fluororesin and polyolefin filters are stored; A method for producing a photoresist liquid product comprising performing the following steps (a) to (d) using an apparatus comprising a pipe connecting the mixing tank, the valve and the filter housing.
(A) filtering the raw material photoresist solution prepared in the mixing tank in a filter housing;
(B) Next, the step of cleaning the inside of the apparatus from the mixing tank to the filter housing inlet with N-methylpyrrolidone, which may contain a solvent component miscible with N-methylpyrrolidone ,
(C) a step of washing one or more wet filters obtained in step (a) using the washing liquid obtained in step (b) in a direction opposite to the direction during filtration;
(D) The step of filtering the same or different raw photoresist liquid as the raw photoresist liquid in the step (a) with the filter back-washed in the step (c):
However, when the raw material photoresist solution to be filtered in the step (d) is different from the raw material photoresist solution in the step (a), the solvents constituting the both photoresist solutions are the same.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001115092A JP3832268B2 (en) | 2001-04-13 | 2001-04-13 | Photoresist liquid product manufacturing method |
| US10/117,248 US7264912B2 (en) | 2001-04-13 | 2002-04-08 | Method of producing photoresist |
| KR1020020019381A KR20020092170A (en) | 2001-04-13 | 2002-04-10 | Process for preparation of photoresist |
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| JP2001115092A JP3832268B2 (en) | 2001-04-13 | 2001-04-13 | Photoresist liquid product manufacturing method |
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| JP3832268B2 true JP3832268B2 (en) | 2006-10-11 |
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