JP2000265151A - Temporary liquid adhesive - Google Patents

Temporary liquid adhesive

Info

Publication number
JP2000265151A
JP2000265151A JP11071263A JP7126399A JP2000265151A JP 2000265151 A JP2000265151 A JP 2000265151A JP 11071263 A JP11071263 A JP 11071263A JP 7126399 A JP7126399 A JP 7126399A JP 2000265151 A JP2000265151 A JP 2000265151A
Authority
JP
Japan
Prior art keywords
acid value
weight
alkali
wafer
softening point
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP11071263A
Other languages
Japanese (ja)
Other versions
JP4492893B2 (en
Inventor
Kyoichi Yamamoto
恭一 山本
Koujun Uko
公淳 宇高
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Inctec Inc
Original Assignee
Inctec Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Inctec Inc filed Critical Inctec Inc
Priority to JP07126399A priority Critical patent/JP4492893B2/en
Publication of JP2000265151A publication Critical patent/JP2000265151A/en
Application granted granted Critical
Publication of JP4492893B2 publication Critical patent/JP4492893B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Abstract

PROBLEM TO BE SOLVED: To provide a temporary liquid adhesive which maintains alkali cleansability and does not cause the flotation of a wafer, when the wafer is subjected to a mirror surface polishing treatment in a polishing process, and has an excellent adhesive strength. SOLUTION: This temporary liquid adhesive comprises an alkali-soluble resin having an acid value of >=60 mgKOH/g and a slightly alkali-soluble resin having an acid value of <=60 mgKOH/g in an amount of <30 wt.% based on the alkali-soluble resin. The alkali-soluble resin is especially an alkali-soluble resin having an acid value of >=120 mgKOH/g.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【発明の属する技術分野】本発明は、半導体ウエハ、化
合物半導体ウエハ等の鏡面研磨加工に際し、研磨定盤と
ウエハを仮着固定する液状仮着接着剤に関するものであ
る。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a liquid temporary adhesive for temporarily fixing a polishing platen and a wafer in mirror polishing of a semiconductor wafer, a compound semiconductor wafer or the like.

【0001】[0001]

【従来の技術】最近の高密度化された半導体ウエハ、化
合物半導体ウエハ等における鏡面研磨加工にあっては、
ウエハ面或いは研磨用定盤に液状仮着接着剤を塗工・乾
燥後、熱圧でウエハと研磨用定盤を接着固定し、ポリシ
ング工程によりウエハの鏡面研磨し、次いでウエハ剥離
−アルカリ洗浄−純水洗浄−乾燥工程を経る。
2. Description of the Related Art Mirror polishing of recent high-density semiconductor wafers, compound semiconductor wafers, etc.
After applying and drying the liquid temporary adhesive on the wafer surface or the polishing surface plate, the wafer and the polishing surface plate are bonded and fixed by heat and pressure, and the wafer is mirror-polished by a polishing process, and then the wafer peeling-alkali cleaning- Through pure water washing and drying process.

【0002】しかしながら、ポリシング工程におけるウ
エハの鏡面研磨に際して、研磨液としてアルカリ研磨液
が使用されるが、仮着接着剤のアルカリ溶解性が強すぎ
ると鏡面加工時にウエハの外周部より研磨液が侵食し、
ウエハの浮きが生じ、場合によっては研磨作業が続行不
可能となる等の問題がある。
However, when polishing the mirror surface of the wafer in the polishing step, an alkaline polishing solution is used as a polishing solution. If the alkali solubility of the temporary adhesive is too strong, the polishing solution erodes from the outer peripheral portion of the wafer during mirror polishing. And
There is a problem that the wafer is lifted, and in some cases, the polishing operation cannot be continued.

【0003】[0003]

【発明が解決しようとする課題】本発明の目的は、ポリ
シング工程におけるウエハの鏡面研磨に際して、アルカ
リ洗浄性を維持しつつもウエハの浮きを生じることな
く、また、接着強度も優れた液状仮着接着剤の提供にあ
る。
SUMMARY OF THE INVENTION It is an object of the present invention to provide a liquid temporary deposition which maintains the alkaline cleaning property without causing the wafer to float, and has an excellent adhesive strength when the wafer is mirror-polished in a polishing step. In providing adhesives.

【0004】[0004]

【課題を解決するための手段】本発明の液状仮着接着剤
は、酸価が60mgKOH/g以上のアルカリ可溶性樹
脂と、該アルカリ可溶性樹脂に対して30重量%未満の
割合の酸価が60mgKOH/g未満のアルカリ難溶性
樹脂とからなることを特徴とする。
The liquid temporary adhesive of the present invention comprises an alkali-soluble resin having an acid value of 60 mg KOH / g or more, and an acid value of less than 30% by weight based on the alkali-soluble resin. / G of less-soluble alkali-soluble resin.

【0005】[0005]

【発明の実施の形態】以下、本発明の液状仮着接着剤に
ついて説明する。本発明におけるアルカリ可溶性樹脂
は、酸価が60mgKOH/g以上、好ましくは120
mgKOH/g以上であり、例えば荒川化学工業(株)
製白菊ロジン(軟化点78℃、酸価165mgKOH/
g)、ハーキュレス(株)製「ウッドロジンWG」(軟
化点78℃、酸価165mgKOH/g)等のロジン
類、東都化成(株)製AX311M(軟化点90℃、酸
価120mgKOH/g)等のノボラック型エポキシ樹
脂、荒川化学工業(株)製(軟化点125℃、酸価24
0mgKOH/g)のアクリル酸変性ロジン、ジョンソ
ンポリマー(株)製(軟化点105℃、酸価238mg
KOH/g)のスチレン−マレイン酸樹脂、日立化成
(株)製「テスポール1155」軟化点130℃、酸価
180mgKOH/g)等のロジン変性マレイン酸樹
脂、岐阜シエラック(株)製「商品名、セラックGS」
(軟化点76℃、接着力62kg/cm2 )、興洋化学
(株)製「商品名、セラックHK」(軟化点75℃、接
着力64.5kg/cm2 )等の酸価65〜80mgK
OH/gの天然シェラック樹脂、合成シェラック樹脂等
が挙げられる。
DESCRIPTION OF THE PREFERRED EMBODIMENTS The liquid temporary adhesive of the present invention will be described below. The alkali-soluble resin in the present invention has an acid value of 60 mgKOH / g or more, preferably 120 mgKOH / g or more.
mgKOH / g or more, for example, Arakawa Chemical Industry Co., Ltd.
Shiragiku Rosin (softening point 78 ° C, acid value 165mgKOH /
g), rosins such as “Wood Rosin WG” (softening point 78 ° C., acid value 165 mg KOH / g) manufactured by Hercules Co., Ltd .; AX311M (softening point 90 ° C., acid value 120 mg KOH / g) manufactured by Toto Kasei Co., Ltd. Novolak type epoxy resin, manufactured by Arakawa Chemical Industry Co., Ltd. (softening point 125 ° C, acid value 24
0 mgKOH / g) acrylic acid-modified rosin (manufactured by Johnson Polymer Co., Ltd. (softening point 105 ° C., acid value 238 mg)
Styrene-maleic resin such as KOH / g), rosin-modified maleic resin such as "Tespol 1155" manufactured by Hitachi Chemical Co., Ltd., having a softening point of 130 ° C and an acid value of 180 mgKOH / g); Shellac GS "
(Softening point of 76 ℃, the adhesive strength 62kg / cm 2), Kyoyo Chemical Co., Ltd. "product name, shellac HK" (softening point of 75 ℃, the adhesive force 64.5kg / cm 2) acid value of such 65~80mgK
OH / g natural shellac resin, synthetic shellac resin and the like.

【0006】アルカリ可溶性樹脂における軟化点は、基
材の材質やユーザー要望等により適宜調整されるが、4
0℃〜100℃、好ましくは50℃〜90℃である。ア
ルカリ可溶性樹脂における酸価が60mgKOH/gよ
り低いと、アルカリ洗浄性に劣るものとなる。
[0006] The softening point of the alkali-soluble resin is appropriately adjusted according to the material of the base material and the user's demand.
0 ° C to 100 ° C, preferably 50 ° C to 90 ° C. If the acid value of the alkali-soluble resin is lower than 60 mgKOH / g, the alkali-cleaning properties will be poor.

【0007】また、アルカリ難溶性樹脂としては、酸価
が60mgKOH/g未満、好ましくは50mgKOH
/g以下であり、例えば荒川化学工業(株)製「エステ
ルガムKE311」(軟化点95℃、酸価10mgKO
H/g)、ハーキュレス(株)製「エステルガムRE」
(軟化点90℃、酸価7mgKOH/g)等のロジンエ
ステル類、ジョンソンポリマー(株)製「ジョンクリル
611」(軟化点112℃、酸価53mgKOH/
g)、野田ワックス(株)製「キャンデリラワックス」
(軟化点70℃、酸価20mgKOH/g)、ヘキスト
ジャパン(株)製ヘキストワックスE(軟化点80℃、
酸価20mgKOH/g)等の天然または合成ワック
ス、野田ワックス(株)製「脱臭精密蜜蝋(高酸)」
(軟化点67℃、酸価20mgKOH/g)、三木化学
工業(株)製「脱臭赤印晒密蝋」(軟化点64℃、酸価
7mgKOH/g)等の蜜蝋、昭和高分子工業(株)製
「PR300」(軟化点60℃、酸価50mgKOH/
g)等のノボラックエポキシアクリレートが例示され
る。また、酸価が60mgKOH/g未満の酢酸ビニル
マレイン酸樹脂を使用してもよい。アルカリ難溶性樹脂
における酸価が60mgKOH/g以上であると、アル
カリ研磨に際してウエハ端面からの侵食性に劣るものと
なる。また、アルカリ難溶性樹脂における軟化点は40
℃〜110℃、好ましくは50℃〜80℃である。
[0007] The hardly soluble alkali resin has an acid value of less than 60 mgKOH / g, preferably 50 mgKOH / g.
/ G or less, for example, “Ester Gum KE311” manufactured by Arakawa Chemical Industry Co., Ltd. (softening point 95 ° C., acid value 10 mg KO
H / g), Hercules Co., Ltd. “Ester gum RE”
Rosin esters such as (softening point 90 ° C., acid value 7 mg KOH / g) and “Johncryl 611” manufactured by Johnson Polymer Co. (softening point 112 ° C., acid value 53 mg KOH / g)
g), "Candelilla wax" manufactured by Noda Wax Co., Ltd.
(Softening point 70 ° C, acid value 20 mg KOH / g), Hoechst Wax E manufactured by Hoechst Japan Co., Ltd. (softening point 80 ° C,
Natural or synthetic wax with an acid value of 20 mg KOH / g, etc., "Deodorized precision beeswax (high acid)" manufactured by Noda Wax Co., Ltd.
(Softening point 67 ° C., acid value 20 mg KOH / g), beeswax such as “Deodorized red seal bleached wax” (softening point 64 ° C., acid value 7 mg KOH / g) manufactured by Miki Chemical Industry Co., Ltd., Showa Kogyo Kogyo Co., Ltd. "PR300" (softening point 60 ° C, acid value 50mgKOH /
g) and the like. Further, a vinyl maleate resin having an acid value of less than 60 mgKOH / g may be used. If the acid value of the poorly alkali-soluble resin is 60 mgKOH / g or more, the erosion from the wafer end surface during alkali polishing is poor. The softening point of the hardly soluble alkali resin is 40.
C. to 110C, preferably 50C to 80C.

【0008】アルカリ難溶性樹脂は、アルカリ可溶性樹
脂に対して、30重量%未満、好ましくは10重量%〜
25重量%の割合で混合されるとよい。30重量%以上
の含有量であると、アルカリ洗浄性に劣るものとなる。
[0008] The alkali-soluble resin is less than 30% by weight, preferably 10% by weight, based on the alkali-soluble resin.
It may be mixed at a ratio of 25% by weight. When the content is 30% by weight or more, the alkali cleaning property is poor.

【0009】また、本発明の液状仮着接着剤には、トル
エンスルホン酸エチルアミド、フタル酸エステル系化合
物、オキシ酸エステル系化合物およびマレイン酸樹脂等
の脂肪族二塩基酸エステル系化合物、オレイン酸、レシ
チン、脂肪酸アミド、流動性パラフィン等の軟化点調整
剤や溶融粘度調整剤、弗素系界面活性剤等のレベリング
剤、酸化防止剤を添加してもよく、いずれも、アルカリ
可溶性樹脂100重量部に対して20重量部以下、好ま
しくは3重量部〜15重量部の割合でそれぞれ添加され
る。
[0009] The liquid temporary adhesive of the present invention includes an aliphatic dibasic acid ester compound such as toluenesulfonic acid ethylamide, phthalic acid ester compound, oxyacid ester compound and maleic acid resin, oleic acid, Lecithin, fatty acid amide, softening point regulators such as liquid paraffin, melt viscosity regulators, leveling agents such as fluorine-based surfactants, and antioxidants may be added, and all are added to 100 parts by weight of the alkali-soluble resin. 20 parts by weight or less, preferably 3 parts by weight to 15 parts by weight, respectively.

【0010】上記の各成分は、溶媒に溶解されて液状仮
着接着剤とされるが、溶媒としては、各成分に対して溶
解性を有するものであれば使用できるが、n−プロピル
アルコール/トルエン(重量比、3/7)混合溶媒等の
共沸系溶剤を使用するとよい。共沸溶媒系は塗膜中より
スムーズな溶剤脱離性があり、残留溶剤量を著しく少な
くできるので、研磨定盤とウエハ熱貼りに際して残留溶
剤の発泡によるウエハ研磨面の歪みを防止でき、かつ接
着安定性を保持することを可能とする。液状仮着接着剤
は、固型分濃度15%〜50%、好ましくは20%〜4
0%の溶液とされる。
Each of the above components is dissolved in a solvent to form a liquid temporary adhesive. As the solvent, any solvent can be used as long as it has solubility for each component. It is preferable to use an azeotropic solvent such as a mixed solvent of toluene (weight ratio: 3/7). The azeotropic solvent system has a smoother solvent desorption property than in the coating film and can significantly reduce the amount of the residual solvent, so that it is possible to prevent distortion of the polished surface of the wafer due to foaming of the residual solvent when the polishing platen and the wafer are thermally bonded, and Adhesive stability can be maintained. The liquid temporary adhesive has a solid content of 15% to 50%, preferably 20% to 4%.
0% solution.

【0011】本発明の液状仮着接着剤は、ウエハまたは
研磨用定盤上に、スピンコータ、ディップコーター等を
使用して塗布され、溶媒が除去された後、ウエハと研磨
用定盤とが熱圧着されることにより、ウエハは定盤上等
に確実に固定され、次いで、アルカリ研磨液による研磨
加工等が施され、加工後にはスクレバー、ナイフ等を利
用して定盤上等から剥離される。
The liquid temporary adhesive of the present invention is applied on a wafer or a polishing plate using a spin coater, a dip coater or the like, and after the solvent is removed, the wafer and the polishing plate are heated. By being press-bonded, the wafer is securely fixed on the surface plate or the like, and then subjected to a polishing process or the like with an alkaline polishing solution, and after processing, is separated from the surface plate or the like using a screver, a knife, or the like. .

【0012】本発明の液状仮着接着剤を使用して定盤上
に固定されたウエハは、アルカリ研磨液として、通常の
研磨液、例えばローデル・ニッタ(株)製研磨剤「ナル
コ2360」等を使用して研磨される。
The wafer fixed on the surface plate using the liquid temporary adhesive of the present invention can be used as an alkaline polishing liquid, for example, a normal polishing liquid, for example, a polishing agent "Narco 2360" manufactured by Rodel Nitta Co., Ltd. Polished using

【0013】本発明の液状仮着接着剤は、ウエハと定盤
等との接着固定を図り、研磨時における40℃〜50℃
の昇温やアルカリ研磨液に耐え、鏡面研磨に適するもの
であり、研磨加工後には、例えばカミソリの刃先をウエ
ハの接着面に挿入し、一挙に剥離できる。また、剥離さ
れたウエハに付着している接着剤は、一次洗浄をアルカ
リ性の洗浄剤で、次いで仕上げリンスを純水で行うこと
により除去される。
The liquid temporary adhesive of the present invention is used for bonding and fixing a wafer to a surface plate and the like, and is used at 40 ° C. to 50 ° C. during polishing.
It is resistant to temperature rise and alkali polishing liquid, and is suitable for mirror polishing. After polishing, for example, a razor blade can be inserted into the bonding surface of the wafer and can be peeled off at once. Further, the adhesive adhering to the peeled wafer is removed by performing primary cleaning with an alkaline cleaning agent and then performing final rinsing with pure water.

【0014】ウエハに残留した接着剤は、テトラメチル
アンモニウムオキサイド、アルカノールアミン、アミノ
アルコール、水溶性アミン類等の有機アミン、無機アル
カリ、またはこれらの塩の水溶液を使用して洗浄除去さ
れる。次に、本発明を実施例および比較例により具体的
に説明する。
The adhesive remaining on the wafer is washed and removed using an aqueous solution of an organic amine such as tetramethylammonium oxide, alkanolamine, amino alcohol, or water-soluble amine, an inorganic alkali, or a salt thereof. Next, the present invention will be specifically described with reference to Examples and Comparative Examples.

【0015】[0015]

【実施例1】下記の組成 ・ ロジン(荒川化学工業(株)製「白菊ロジン」軟化点78℃、酸価165m gKOH/g) ・・・・・ 80重量部 ・ 野田ワックス(株)製「脱臭精密蜜蝋(高酸)」(軟化点67℃、酸価20 mgKOH/g) ・・・・・ 10重量部 ・ 荒川化学工業(株)製「エステルガムKE311」(軟化点95℃、酸価1 0mgKOH/g) ・・・・・ 10重量部 からなる組成を、n−プロピルアルコール/トルエン=
3/7(重量比)の混合溶媒に30%固形分濃度で溶解
させ、本発明の液状仮着接着剤を調製した。
Example 1 The following composition: Rosin ("Shiragiku Rosin" manufactured by Arakawa Chemical Industry Co., Ltd., softening point 78 ° C, acid value 165 mg KOH / g) 80 parts by weight Noda Wax Co., Ltd. "Deodorized precision beeswax (high acid)" (softening point 67 ° C, acid value 20 mgKOH / g) 10 parts by weight "Arakawa Chemical Industry Co., Ltd.""Ester gum KE311" (softening point 95 ° C, acid value 10 mg KOH / g) A composition consisting of 10 parts by weight was converted into n-propyl alcohol / toluene =
It was dissolved at a solid content of 30% in a 3/7 (weight ratio) mixed solvent to prepare a liquid temporary adhesive of the present invention.

【0016】[0016]

【実施例2】下記の組成 ・ ハーキュレス(株)製「ウッドロジン」(軟化点78℃、酸価165mgK OH/g) ・・・・・ 80重量部 ・ ハーキュレス(株)製「エステルガムRE」(軟化点90℃、酸価7mgK OH/g) ・・・・・ 10重量部 ・ 野田ワックス(株)製「脱臭精密蜜蝋(高酸)」(軟化点67℃、酸価20 mgKOH/g) ・・・・・ 10重量部 からなる組成を、n−プロピルアルコール/トルエン=
3/7(重量比)の混合溶媒に30%固形分濃度で溶解
させ、本発明の液状仮着接着剤を調製した。
Example 2 The following composition: "Wood Rosin" manufactured by Hercules Co., Ltd. (softening point: 78 ° C., acid value: 165 mgK OH / g) ... 80 parts by weight "Ester Gum RE" manufactured by Hercules Co., Ltd. Softening point 90 ° C, acid value 7 mgK OH / g) 10 parts by weight Noda Wax Co., Ltd. “Deodorized precision beeswax (high acid)” (softening point 67 ° C, acid value 20 mgKOH / g) ... A composition consisting of 10 parts by weight is converted into n-propyl alcohol / toluene =
It was dissolved at a solid content of 30% in a 3/7 (weight ratio) mixed solvent to prepare a liquid temporary adhesive of the present invention.

【0017】[0017]

【実施例3】下記の組成 ・ ハーキュレス(株)製「ウッドロジン」(軟化点78℃、酸価165mgK OH/g) ・・・・・ 40重量部 ・ 日立化成(株)製「テスポール1155」軟化点130℃、酸価180mg KOH/g) ・・・・・ 40重量部 ・ 荒川化学工業(株)製「エステルガムRE」(軟化点90℃、酸価7mgK OH/g) ・・・・・ 10重量部 ・ 荒川化学工業(株)製「エステルガムKE311」(軟化点95℃、酸価1 0mgKOH/g) ・・・・・ 10重量部 からなる組成を、n−プロピルアルコール/トルエン=
3/7(重量比)の混合溶媒に30%固形分濃度で溶解
させ、本発明の液状仮着接着剤を調製した。
Example 3 The following composition: "Wood Rosin" manufactured by Hercules Co., Ltd. (softening point: 78 DEG C., acid value: 165 mgK OH / g) ... 40 parts by weight-"Tespol 1155" manufactured by Hitachi Chemical Co., Ltd. Point 130 ° C, acid value 180 mg KOH / g) 40 parts by weight Arakawa Chemical Industries, Ltd. “Ester gum RE” (softening point 90 ° C, acid value 7 mgKOH / g) 10 parts by weight-"Ester gum KE311" manufactured by Arakawa Chemical Industry Co., Ltd. (softening point: 95 ° C, acid value: 10 mgKOH / g) ... 10 parts by weight of n-propyl alcohol / toluene =
It was dissolved at a solid content of 30% in a 3/7 (weight ratio) mixed solvent to prepare a liquid temporary adhesive of the present invention.

【0018】[0018]

【比較例1】下記の組成 ・ ロジン(荒川化学工業(株)製「白菊ロジン」軟化点78℃、酸価165m gKOH/g) ・・・・・ 60重量部 ・ ハーキュレス(株)製「エステルガムRE」(軟化点90℃、酸価7mgK OH/g) ・・・・・ 20重量部 ・ 荒川化学工業(株)製「エステルガムKE311」(軟化点95℃、酸価1 0mgKOH/g) ・・・・・ 20重量部 ・ オレイン酸(試薬、和光純薬、液状) ・・ 3重量部 からなる組成を、n−プロピルアルコール/トルエン=
3/7(重量比)の混合溶媒に30%固形分濃度で溶解
させ、液状仮着接着剤を調製した。
[Comparative Example 1] The following composition: Rosin ("Shiragiku Rosin" manufactured by Arakawa Chemical Industries, Ltd., softening point 78 ° C, acid value 165 mg KOH / g) ... 60 parts by weight-Hercules "Ester" Gum RE "(softening point 90 ° C, acid value 7mgK OH / g) 20 parts by weight" Arakawa Chemical Industries Co., Ltd. "" Ester gum KE311 "(softening point 95 ° C, acid value 10mgKOH / g) 20 parts by weight Oleic acid (reagent, Wako Pure Chemicals, liquid) 3 parts by weight of n-propyl alcohol / toluene =
It was dissolved in a 3/7 (weight ratio) mixed solvent at a solid content of 30% to prepare a liquid temporary adhesive.

【0019】[0019]

【比較例2】下記の組成 ・ ロジン(荒川化学工業(株)製「白菊ロジン」軟化点78℃、酸価165m gKOH/g) ・・・・・ 70重量部 ・ ハーキュレス(株)製「エステルガムRE」(軟化点90℃、酸価7mgK OH/g) ・・・・・ 15重量部 ・ 野田ワックス(株)製「脱臭精密蜜蝋(高酸)」(軟化点67℃、酸価20 mgKOH/g) ・・・・・ 15重量部 からなる組成を、メチルエチルケトン/トルエン=2/
1(重量比)の混合溶媒に30%固形分濃度で溶解さ
せ、液状仮着接着剤を調製した。
[Comparative Example 2] The following composition: Rosin ("Shiragiku Rosin" manufactured by Arakawa Chemical Industries, Ltd., softening point 78 ° C, acid value 165 mg KOH / g) 70 parts by weight Hercules "Ester" Gum RE "(softening point 90 ° C, acid value 7 mgK OH / g) ... 15 parts by weight" No dewax Co., Ltd. deodorized precision beeswax (high acid) "(softening point 67 ° C, acid value 20 mgKOH) / G) ············· 15 parts by weight of methyl ethyl ketone / toluene = 2 /
It was dissolved in 1 (weight ratio) of the mixed solvent at a solid content of 30% to prepare a liquid temporary adhesive.

【0020】[0020]

【比較例3】下記の組成 ・ ロジン(荒川化学工業(株)製「白菊ロジン」軟化点78℃、酸価165m gKOH/g) ・・・・・ 100重量部 ・ オレイン酸(試薬、和光純薬製、液状)・・・ 5重量部 からなる組成を、メチルエチルケトン/トルエン=2/
1(重量比)の混合溶媒に30%固形分濃度で溶解さ
せ、液状仮着接着剤を調製した。 (アルカリ洗浄性についての評価)上記で得られた実施
例1〜3、比較例1〜3の各液状仮着接着剤に、ワック
ス100gあたり1mgの割合でセレスブルー染料
(C.I.No61520)を添加し、評価用試料とし
た。
[Comparative Example 3] Rosin ("Shiragiku Rosin" manufactured by Arakawa Chemical Industries, Ltd., softening point 78 ° C, acid value 165 mg KOH / g) 100 parts by weight Oleic acid (reagent, Wako Pure) 5 parts by weight of methyl ethyl ketone / toluene = 2 /
It was dissolved in 1 (weight ratio) of the mixed solvent at a solid content of 30% to prepare a liquid temporary adhesive. (Evaluation of Alkali Detergency) To each of the liquid temporary adhesives obtained in Examples 1 to 3 and Comparative Examples 1 to 3 obtained above, a Ceres blue dye (CI No. 61520) was added at a rate of 1 mg per 100 g of wax. Was added to obtain a sample for evaluation.

【0021】ガラスウエハー上にスピンコーターで各評
価用試料を回転塗布した後、熱風乾燥し、乾燥膜厚3±
0.5μmの着色接着剤層を形成し、八角形(対角長5
0mm)の評価用チップを切り出し、図1に示す洗浄装
置に装填した。
Each sample for evaluation was spin-coated on a glass wafer with a spin coater, dried with hot air, and dried to a film thickness of 3 ± 10%.
A 0.5 μm colored adhesive layer is formed, and an octagon (5 mm diagonal)
(0 mm) was cut out and loaded into the cleaning device shown in FIG.

【0022】図1に示す洗浄装置は、300mlビーカ
ー1、攪拌子2、ポリプロピレン製固定台3、評価用チ
ップ支持台4からなり、評価用チップ5を接着剤層7を
下向きにして評価用チップ支持台4に支持させる。ビー
カー内にテトラメチルアンモニウムハイドロオキサイド
25%水溶液(東洋合成工業(株)製「TMAH−25
H」を純水で希釈し、0.2%濃度液とした洗浄液を2
00ml入れ、マグネティックスターラー(Yamat
o Mag−Mixer MD200)上に載置し、液
温40℃において、攪拌速度を最低として洗浄液を攪拌
し、着色接着剤層が全て溶解する時間を測定した。その
結果を下記の表1に示す。表中、1分以内で溶解したも
のを良好、3分以上要したものを不良とした。 (接着強度の測定)2枚1組の測定用治具に試料を塗布
乾燥させ、貼り合わせる(SUS/試料/SUS)。1
00gの重りを乗せて接着させる。25℃のウォーター
バスに1時間入れ、温度を安定させた後、ストログラフ
を使用して引っ張り剪断剥離強度を測定し、接着力(k
g/cm2 )とした。 (端面侵食性の評価法)シリコウエハ(3吋φ、450
μm厚のラッピングウエハ)に、実施例1〜3、比較例
1〜3の各液状仮着接着剤をスピンコートし、乾燥膜厚
3±0.2μmの接着剤層を形成した。この接着剤層側
を研磨用定盤上に合わせ、ホットプレート(150℃)
上で加圧接着させた。
The cleaning device shown in FIG. 1 comprises a 300 ml beaker 1, a stirrer 2, a polypropylene fixing table 3, and an evaluation chip support 4, and the evaluation chip 5 is placed with the adhesive layer 7 facing downward. The support table 4 is supported. In a beaker, a 25% aqueous solution of tetramethylammonium hydroxide (“TMAH-25” manufactured by Toyo Gosei Co., Ltd.)
H "was diluted with pure water to obtain a 0.2% concentration washing solution.
00ml, magnetic stirrer (Yamat
o Mag-Mixer MD200), the washing liquid was stirred at a liquid temperature of 40 ° C. at a minimum stirring speed, and the time required for all the colored adhesive layer to dissolve was measured. The results are shown in Table 1 below. In the table, those dissolved within 1 minute were regarded as good, and those requiring 3 minutes or more as defective. (Measurement of Adhesive Strength) A sample is applied to a set of two measuring jigs, dried, and bonded (SUS / sample / SUS). 1
A weight of 00 g is placed and adhered. After placing in a water bath at 25 ° C. for 1 hour to stabilize the temperature, the tensile shearing peel strength was measured using a strograph, and the adhesive strength (k
g / cm 2 ). (Evaluation method for edge erosion) Silicon wafer (3 inchφ, 450
Each of the liquid temporary adhesives of Examples 1 to 3 and Comparative Examples 1 to 3 was spin-coated on a μm-thick lapping wafer) to form an adhesive layer having a dry film thickness of 3 ± 0.2 μm. Place the adhesive layer side on the polishing platen and hot plate (150 ° C)
The above was pressure-bonded.

【0023】別途、研磨装置(ナノテックマシーンズ製
「 NANOTECH450-FODC 」)に研磨布(SUBA800)
をセッティングした後、研磨剤(ナルコ2360)を研
磨定盤に接着したウエハ面に全面に吹付け、加圧200
g/cm2 、回転数40rpm、研磨時間20分でポリ
ッシングした。なお、研磨剤の供給は5分間隔で実施し
た。鏡面研磨完了後、ウエハを剥離し、ウエハ端面の研
磨液侵食長(外周部から中心部までの研磨液侵食長)を
計測した。その結果を同じく、表1に示す。なお、表
中、7mm以上研磨剤に侵食されたもの×、3mm以内
を○とし、中程度を○〜△とした。 (残留溶剤量評価法)シリコンウエハ(3吋φ、450
μm厚のラッピングウエハ)に、実施例1〜3及び比較
例1〜3で試作した液状仮着接着剤をスピンコーターに
より3±0.2μmの膜厚に塗工した後、ホットプレー
ト上で100℃、6秒間熱乾し、試料とした。試料を細
片化し、大型試験管に一定量封入した後、120℃、1
0分間オーブン中で加熱して残留溶剤を追い出し、大型
試験管内における溶剤量をガスクロマトグラフィ法で定
量し、3吋φウエハ一枚当りに換算した値(mg/3吋
φ)を表1に示す。
Separately, a polishing cloth (SUBA800) is mounted on a polishing apparatus ("NANOTECH450-FODC" manufactured by Nanotech Machines).
After setting, the abrasive (Narco 2360) is sprayed over the entire surface of the wafer adhered to the polishing platen,
Polishing was performed at g / cm 2 , rotation speed of 40 rpm, and polishing time of 20 minutes. The supply of the abrasive was performed at intervals of 5 minutes. After the mirror polishing was completed, the wafer was peeled off, and the polishing liquid erosion length (the polishing liquid erosion length from the outer peripheral portion to the center portion) of the wafer end surface was measured. Table 1 also shows the results. In the table, those eroded by the abrasives of 7 mm or more × were within 3 mm, and ○ were given, and the medium was given as △ to Δ. (Residual solvent amount evaluation method) Silicon wafer (3 inchφ, 450
The liquid temporary adhesive prepared in Examples 1 to 3 and Comparative Examples 1 to 3 was applied to a thickness of 3 ± 0.2 μm on a wrapping wafer having a thickness of 3 μm by a spin coater, and then 100 μm on a hot plate. The sample was dried by heating at 6 ° C. for 6 seconds. After shredding the sample into small pieces and enclosing a fixed amount in a large test tube,
The residual solvent was driven out by heating in an oven for 0 minutes, the amount of the solvent in the large test tube was quantified by gas chromatography, and the value (mg / 3 inch φ) converted per wafer of 3 inch φ is shown in Table 1. .

【0024】[0024]

【表1】 [Table 1]

【0025】[0025]

【実施例4】下記の組成 ・ シェラック樹脂(岐阜セラック(株)製「PN−M60」、60%メタノー ル液)(軟化点75℃、酸価80mgKOH/g) ・・・・・ 30重量部 ・ 酢酸ビニル樹脂(積水化学(株)製「エスニールC−2」)(軟化点42℃ 、酸価0mgKOH/g) ・・・・・ 10重量部 ・ オレイン酸(試薬、和光純薬製、液状)・・・ 2重量部 ・ 変性エタノール ・・・・・ 30重量部 ・ 酢酸エチル ・・・・・ 28重量部 からなる組成の本発明の液状仮着接着剤を調製した。Example 4 The following composition: Shellac resin ("PN-M60" manufactured by Gifu Shellac Co., Ltd., 60% methanol solution) (softening point: 75 ° C., acid value: 80 mg KOH / g) 30 parts by weight・ Vinyl acetate resin (“Sneil C-2” manufactured by Sekisui Chemical Co., Ltd.) (softening point: 42 ° C., acid value: 0 mg KOH / g) 10 parts by weight ・ Oleic acid (reagent, manufactured by Wako Pure Chemical, liquid) ) ... 2 parts by weight-denatured ethanol ... 30 parts by weight-ethyl acetate ... 28 parts by weight A liquid temporary adhesive of the present invention having a composition of 28 parts by weight was prepared.

【0026】[0026]

【実施例5】下記の組成 ・ シェラック樹脂(岐阜セラック(株)製「PN−M60」、60%メタノー ル液)(軟化点75℃、酸価80mgKOH/g) ・・・・・ 35重量部 ・ 酢酸ビニルマレイン酸樹脂(興洋化学(株)製「THR」)(軟化点60℃ 、酸価50mgKOH/g) ・・・・・ 7重量部 ・ オレイン酸(試薬、和光純薬製、液状)・・・ 2重量部 ・ 変性エタノール ・・・・・ 30重量部 ・ 酢酸エチル ・・・・・ 26重量部 からなる組成の本発明の液状仮着接着剤を調製した。Example 5 The following composition: Shellac resin ("PN-M60" manufactured by Gifu Shellac Co., Ltd., 60% methanol solution) (softening point: 75 ° C., acid value: 80 mg KOH / g) 35 parts by weight・ Vinyl acetate maleate resin (“THR” manufactured by Koyo Chemical Co., Ltd.) (softening point 60 ° C., acid value 50 mg KOH / g) 7 parts by weight ・ Oleic acid (reagent, manufactured by Wako Pure Chemical, liquid ) ... 2 parts by weight-denatured ethanol ... 30 parts by weight-ethyl acetate ... 26 parts by weight A liquid temporary adhesive of the present invention having a composition of 26 parts by weight was prepared.

【0027】[0027]

【実施例6】下記の組成 ・ シェラック樹脂(岐阜セラック(株)製「PN−M60」、60%メタノー ル液)(軟化点75℃、酸価80mgKOH/g) ・・・・・ 35重量部 ・ スチレン−マレイン酸樹脂( BASF(株)製「スプラパールAP」)( 軟化点160℃、酸価155mgKOH/g)・・ 7重量部 ・ オレイン酸(試薬、和光純薬製、液状) ・・ 2重量部 ・ 変性エタノール ・・・・ 35重量部 ・ 酢酸エチル ・・・・ 21重量部 からなる組成の本発明の液状仮着接着剤を調製した。Example 6 The following composition: Shellac resin ("PN-M60", Gifu Shellac Co., Ltd., 60% methanol solution) (softening point 75 ° C, acid value 80 mg KOH / g) 35 parts by weight • Styrene-maleic acid resin (“Suprapearl AP” manufactured by BASF) (softening point 160 ° C, acid value 155 mgKOH / g) 7 parts by weight oleic acid (reagent, manufactured by Wako Pure Chemical, liquid) 2 35 parts by weight of denatured ethanol .... 21 parts by weight of ethyl acetate. A liquid temporary adhesive of the present invention having a composition of 21 parts by weight was prepared.

【0028】上記実施例4〜実施例6の液状仮着接着剤
について、上記実施例1〜3と同様の評価を行った。そ
の結果を表2に示す。
With respect to the liquid temporary adhesives of Examples 4 to 6, the same evaluations as in Examples 1 to 3 were performed. Table 2 shows the results.

【0029】[0029]

【表2】 [Table 2]

【0030】[0030]

【発明の効果】本発明の液状仮着接着剤は、ポリシング
工程におけるウエハの鏡面研磨に際して、アルカリ洗浄
性を維持しつつもウエハの浮きを生じることなく、ま
た、接着強度も優れるものである。
The liquid temporary adhesive according to the present invention does not cause the wafer to float while maintaining the alkaline cleaning property during the mirror polishing of the wafer in the polishing step, and has excellent adhesive strength.

【図面の簡単な説明】[Brief description of the drawings]

【図1】 液状仮着接着剤におけるアルカリ洗浄性評価
装置を説明するための図である。
FIG. 1 is a diagram for explaining an apparatus for evaluating the alkali cleaning property of a liquid temporary adhesive.

【符号の説明】[Explanation of symbols]

1は300mlビーカー、2は攪拌子、3はポリプロピ
レン製固定台、4は評価用チップ支持台、5は評価用チ
ップ、6はマグネティックスターラー、7は接着剤層で
ある。
1 is a 300 ml beaker, 2 is a stirrer, 3 is a polypropylene fixing table, 4 is an evaluation chip support, 5 is an evaluation chip, 6 is a magnetic stirrer, and 7 is an adhesive layer.

───────────────────────────────────────────────────── フロントページの続き Fターム(参考) 4J040 BA182 BA191 BA201 BA202 DB041 DE022 DG001 DG041 EC071 FA202 JA02 JB05 LA06 LA08 MA01 MA02 NA20 PA20 PA42  ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 4J040 BA182 BA191 BA201 BA202 DB041 DE022 DG001 DG041 EC071 FA202 JA02 JB05 LA06 LA08 MA01 MA02 NA20 PA20 PA42

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】 酸価が60mgKOH/g以上のアルカ
リ可溶性樹脂と、該アルカリ可溶性樹脂に対して30重
量%未満の割合の酸価が60mgKOH/g以下のアル
カリ難溶性樹脂とからなることを特徴とする液状仮着接
着剤。
1. An alkali-soluble resin having an acid value of 60 mg KOH / g or more, and an alkali-soluble resin having an acid value of less than 30% by weight based on the alkali-soluble resin and having an acid value of 60 mg KOH / g or less. Liquid temporary adhesive.
【請求項2】 アルカリ可溶性樹脂が、酸価120mg
KOH/g以上のアルカリ可溶性樹脂であることを特徴
とする請求項1記載の液状仮着接着剤。
2. An alkali-soluble resin having an acid value of 120 mg.
The liquid temporary adhesive according to claim 1, wherein the adhesive is a KOH / g or more alkali-soluble resin.
JP07126399A 1999-03-17 1999-03-17 Liquid temporary adhesive Expired - Fee Related JP4492893B2 (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009197175A (en) * 2008-02-25 2009-09-03 The Inctec Inc Cleaning agent stock liquid
JP2013014777A (en) * 2008-10-31 2013-01-24 Brewer Science Inc Cyclic olefin compositions for temporary wafer bonding
JP2014036054A (en) * 2012-08-07 2014-02-24 Sumco Corp Single side polishing method of wafer
WO2018101453A1 (en) * 2016-12-01 2018-06-07 株式会社Dnpファインケミカル Temporary adhesive and component manufacturing method
WO2020246470A1 (en) * 2019-06-03 2020-12-10 株式会社Dnpファインケミカル Water-based temporary fixing adhesive, and method for producing various members or parts using said water-based temporary fixing adhesive

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JPH01150493A (en) * 1987-12-08 1989-06-13 Asahi Chem Res Lab Ltd Temporary adhesive for soldering
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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009197175A (en) * 2008-02-25 2009-09-03 The Inctec Inc Cleaning agent stock liquid
JP2013014777A (en) * 2008-10-31 2013-01-24 Brewer Science Inc Cyclic olefin compositions for temporary wafer bonding
JP2014036054A (en) * 2012-08-07 2014-02-24 Sumco Corp Single side polishing method of wafer
WO2018101453A1 (en) * 2016-12-01 2018-06-07 株式会社Dnpファインケミカル Temporary adhesive and component manufacturing method
JP6403935B1 (en) * 2016-12-01 2018-10-10 株式会社Dnpファインケミカル Temporary adhesive and component manufacturing method
WO2020246470A1 (en) * 2019-06-03 2020-12-10 株式会社Dnpファインケミカル Water-based temporary fixing adhesive, and method for producing various members or parts using said water-based temporary fixing adhesive
JP2020196813A (en) * 2019-06-03 2020-12-10 株式会社Dnpファインケミカル Water-based temporary adhesive and method for manufacturing various members or components by using the same
CN113939570A (en) * 2019-06-03 2022-01-14 Dnp精细化工股份有限公司 Aqueous temporary fixing adhesive and method for producing various members or components using same
JP7288807B2 (en) 2019-06-03 2023-06-08 株式会社Dnpファインケミカル Water-based temporary fixing adhesive and method for manufacturing various members or parts using the water-based temporary fixing adhesive
CN113939570B (en) * 2019-06-03 2024-01-05 Dnp精细化工股份有限公司 Aqueous temporary fixing adhesive and method for producing various members or components using same

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