TW201439272A - Adhesive sheet - Google Patents
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本發明係關於一種黏著片材。 The present invention relates to an adhesive sheet.
包含矽、鎵、砷等之半導體晶圓以大直徑狀態製造，於表面形成圖案後研磨背面，通常將晶圓之厚度磨薄至100~600μm左右，進而切割分離(dicing)為元件小片，進一步移送至安裝步驟。 A semiconductor wafer including germanium, gallium, arsenic or the like is manufactured in a large diameter state, and a back surface is formed by patterning the surface, and the thickness of the wafer is usually thinned to about 100 to 600 μm, and then dicing is a small piece of the component, and further Transfer to the installation step.
於研磨半導體晶圓之背面之步驟(背面研磨步驟)中，為了保護半導體晶圓之圖案面而使用黏著片材。該黏著片材通常於背面研磨步驟後被剝離。以此種目的而使用之黏著片材需要有於背面研磨步驟中不會發生剝離之程度的黏著力，另一方面，要求於背面研磨步驟後能夠容易地剝離，而且不損壞半導體晶圓之程度之低黏著力。為了如此調整黏著力，提出具有將2種以上之樹脂(例如，黏著性樹脂及非黏著性樹脂)摻合而形成之黏著劑層的黏著片材(專利文獻1)。 In the step of polishing the back surface of the semiconductor wafer (back grinding step), an adhesive sheet is used to protect the pattern surface of the semiconductor wafer. The adhesive sheet is usually peeled off after the back grinding step. The adhesive sheet used for such a purpose needs to have an adhesive force which does not peel off in the back grinding step, and on the other hand, it is required to be easily peeled off after the back grinding step without damaging the semiconductor wafer. Low adhesion. In order to adjust the adhesive force as described above, an adhesive sheet having an adhesive layer formed by blending two or more kinds of resins (for example, an adhesive resin and a non-adhesive resin) has been proposed (Patent Document 1).
但是，將具有由2種以上之樹脂形成之黏著劑層的黏著片材貼附於半導體晶圓，並將半導體晶圓供於背面研磨步驟之情形時，有此種問題：研磨水及/或研磨屑容易滲入至黏著片材與半導體晶圓之間，有污染半導體晶圓之虞。 However, when an adhesive sheet having an adhesive layer formed of two or more kinds of resins is attached to a semiconductor wafer and the semiconductor wafer is supplied to the back grinding step, there is such a problem that grinding water and/or The abrasive debris easily penetrates between the adhesive sheet and the semiconductor wafer, and is contaminated by the semiconductor wafer.
專利文獻1：日本專利特開2012-62406號公報 Patent Document 1: Japanese Patent Laid-Open Publication No. 2012-62406
本發明係為了解決上述先前課題而成者，其目的在於提供一種黏著片材，其於貼附於半導體晶圓並供於半導體晶圓之背面研磨步驟之情形時，能夠防止研磨水及/或研磨屑滲入至黏著片材與半導體晶圓之間。 The present invention has been made to solve the above problems, and an object thereof is to provide an adhesive sheet capable of preventing grinding water and/or when attached to a semiconductor wafer and supplied to a back surface polishing step of a semiconductor wafer. The abrasive chips penetrate between the adhesive sheet and the semiconductor wafer.
本發明之黏著片材具備包含2種以上之樹脂之黏著劑層，於該黏著劑層中，由利用原子力顯微鏡測定之與被黏著體相接觸側之表面的相位圖像獲得的以縱軸(y軸)為相位差、以橫軸(x軸)為測定距離的第1方向及與該第1方向正交的第2方向的線分佈中，第1方向上之相位差的大小(P1-avg)與第2方向上之相位差的大小(P2-avg)之比(P1-avg/P2-avg)為0.94~1.06。 The adhesive sheet of the present invention comprises an adhesive layer containing two or more kinds of resins, and a longitudinal axis obtained by a phase image of a surface on the side in contact with the adherend body measured by an atomic force microscope in the adhesive layer ( The y-axis is the phase difference, the horizontal direction (x-axis) is the first direction of the measurement distance, and the line direction of the second direction orthogonal to the first direction, the magnitude of the phase difference in the first direction (P 1 ) The ratio of the magnitude of the phase difference (P 2-avg ) between the -avg and the second direction (P 1-avg /P 2-avg ) is 0.94 to 1.06.
於較佳之實施形態中，構成上述黏著劑層之2種以上的樹脂分別具有共通之構成單元作為主要構成單元。 In a preferred embodiment, the two or more kinds of resins constituting the pressure-sensitive adhesive layer each have a common constituent unit as a main constituent unit.
根據本發明，可提供一種黏著片材，其於貼附於半導體晶圓並供於半導體晶圓之背面研磨步驟之情形時，能夠防止研磨水及/或研磨屑滲入至黏著片材與半導體晶圓之間。 According to the present invention, it is possible to provide an adhesive sheet which can prevent the penetration of grinding water and/or abrasive chips into the adhesive sheet and the semiconductor crystal when attached to the semiconductor wafer and supplied to the back grinding step of the semiconductor wafer. Between the circles.
10‧‧‧黏著劑層 10‧‧‧Adhesive layer
20‧‧‧中間層 20‧‧‧Intermediate
30‧‧‧基材層 30‧‧‧Substrate layer
100‧‧‧黏著片材 100‧‧‧Adhesive sheets
圖1係本發明之黏著劑層之由利用原子力顯微鏡之相位圖像而獲得的線分佈。 Fig. 1 is a line distribution of an adhesive layer of the present invention obtained by using a phase image of an atomic force microscope.
圖2係本發明之一個實施形態之黏著片材的概略剖面圖。 Fig. 2 is a schematic cross-sectional view showing an adhesive sheet according to an embodiment of the present invention.
A.黏著劑層 A. Adhesive layer
本發明之黏著片材具備黏著劑層。該黏著劑層包含2種以上之樹脂，較佳為包含至少1種以上之黏著性樹脂及至少1種以上之非黏著性 樹脂。若黏著劑層如此包含2種以上之樹脂，則變得容易調整樹脂之種類及樹脂之含有比例來適當控制黏著力及儲存模數(G')。 The adhesive sheet of the present invention has an adhesive layer. The adhesive layer contains two or more kinds of resins, preferably at least one or more adhesive resins and at least one or more non-adhesive properties. Resin. When the adhesive layer contains two or more kinds of resins as described above, it is easy to adjust the type of the resin and the content ratio of the resin to appropriately control the adhesion and the storage modulus (G').
上述黏著劑層於50℃下老化2天後，將半導體鏡面晶圓(矽製)作為試驗板，利用以JIS Z 0237(2000)為基準之方法(貼合條件：2kg輥往復1次、剝離速度：300mm/min、剝離角度180°)測定之黏著力較佳為0.1N/20mm~3.0N/20mm，進而較佳為0.2N/20mm~2.5N/20mm，特別較佳為0.2N/20mm~2.0N/20mm。若為此種範圍，則能夠兼顧黏著力及剝離性，能夠獲得例如於半導體晶圓之背面研磨步驟中之研磨加工中不剝離，而於研磨加工後能夠容易地剝離之黏著片材。 After the adhesive layer was aged at 50 ° C for 2 days, a semiconductor mirror wafer (manufactured by Nippon Co., Ltd.) was used as a test plate, and a method based on JIS Z 0237 (2000) was used. (Adhesion conditions: 2 kg roller reciprocating once, peeling The adhesive force measured at a speed of 300 mm/min and a peeling angle of 180° is preferably 0.1 N/20 mm to 3.0 N/20 mm, more preferably 0.2 N/20 mm to 2.5 N/20 mm, and particularly preferably 0.2 N/20 mm. ~2.0N/20mm. In such a range, the adhesive force and the peeling property can be achieved at the same time, and an adhesive sheet which can be easily peeled off after the polishing process can be obtained, for example, in the polishing process in the back surface polishing step of the semiconductor wafer.
上述黏著劑層之儲存模數(G')較佳為0.5×106Pa~1.0×108Pa，進而較佳為0.8×106Pa~3.0×107Pa。若上述黏著劑層之儲存模數(G')在此種範圍，則能夠獲得可兼顧對表面具有凹凸之被黏著體之充分的黏著力及適度之剝離性的黏著片材。另外，具備此種儲存模數(G')之上述黏著劑層之黏著片材於用於半導體晶圓加工用之情形時，能夠有助於達成晶圓之背面研磨中之優異的研磨精度。再者，本發明中之儲存模數(G')可藉由動態黏彈性光譜測定來測定。 The storage modulus (G') of the above adhesive layer is preferably from 0.5 × 10 6 Pa to 1.0 × 10 8 Pa, more preferably from 0.8 × 10 6 Pa to 3.0 × 10 7 Pa. When the storage modulus (G') of the pressure-sensitive adhesive layer is in such a range, it is possible to obtain an adhesive sheet which can achieve sufficient adhesion to the adherend having irregularities on the surface and moderate peelability. Further, when the adhesive sheet having the above-described adhesive layer having the storage modulus (G') is used for semiconductor wafer processing, it can contribute to excellent polishing precision in back surface polishing of the wafer. Furthermore, the storage modulus (G') in the present invention can be determined by dynamic viscoelastic spectroscopy.
上述黏著劑層中，由利用原子力顯微鏡測定之與被黏著體相接觸側之表面之相位圖像獲得的以縱軸(y軸)為相位差(利用原子力顯微鏡測定之輸入信號與輸出信號之相位差(°))、以橫軸(x軸)為測定距離之第1方向及與該第1方向正交之第2方向的線分佈中，第1方向上之相位差的大小(P1-avg)與第2方向上之相位差的大小(P2-avg)之比(P1-avg/P2-avg)為0.94~1.06。此處，第1方向上之相位差的大小(P1-avg)係指於上述第1方向之線分佈中，將以第1方向之特定距離L上之相位差平均線為基準的波形面積除以該距離L而獲得之值設為P1(°)，由隨機抽取之128條線獲得之P1的平均值。另外，第2方向上之相位差的大小(P2-avg)係指 上述第2方向之線分佈中，將以第2方向之特定距離L上之相位差平均線為基準的波形面積除以該距離L而獲得的值設為P2(°)，由隨機抽取之128條線獲得之P2的平均值。圖1表示由上述相位圖像獲得之線分佈的一例。另外，P1(°)及P2(°)用下述式(1)表示。上述L例如設定為1μm~10μm，較佳為2μm~5μm，更佳為2.5μm。相位圖像之測定方法於下文進行說明。於一個實施形態中，上述第2方向為平行於製造黏著片材時之搬送方向之方向(MD)，上述第1方向為與MD正交的方向(TD)。 In the above adhesive layer, the longitudinal axis (y-axis) obtained by the phase image of the surface on the side in contact with the adherend measured by an atomic force microscope is a phase difference (the phase of the input signal and the output signal measured by an atomic force microscope) Difference (°)), the horizontal axis (x-axis) is the magnitude of the phase difference in the first direction in the first direction of the measurement distance and the second direction orthogonal to the first direction (P 1- The ratio of the phase difference (P 2-avg ) between the avg and the second direction (P 1-avg /P 2-avg ) is 0.94 to 1.06. Here, the magnitude (P 1-avg ) of the phase difference in the first direction means a waveform area based on the phase difference average line at a specific distance L in the first direction in the line distribution in the first direction. The value obtained by dividing the distance L is set to P 1 (°), and the average value of P 1 obtained from the randomly selected 128 lines. Further, the magnitude (P 2-avg ) of the phase difference in the second direction means that the waveform area based on the phase difference average line at the specific distance L in the second direction is divided by the line distribution in the second direction. The value obtained by this distance L is set to P 2 (°), and the average value of P 2 obtained from the 128 lines randomly selected. Fig. 1 shows an example of a line distribution obtained from the above phase image. Further, P 1 (°) and P 2 (°) are represented by the following formula (1). The above L is, for example, 1 μm to 10 μm, preferably 2 μm to 5 μm, and more preferably 2.5 μm. The method of measuring the phase image is described below. In one embodiment, the second direction is a direction (MD) parallel to a conveying direction when the adhesive sheet is produced, and the first direction is a direction (TD) orthogonal to the MD.
上述P1-avg與P2-avg之比(P1-avg/P2-avg)表示相位圖像之各向異性。(P1-avg/P2-avg)越接近1，則各向異性越低；若為1則可稱為各向同性。根據相位圖像之各向異性能夠推測2種以上之樹脂的混合狀態。具體而言，若相位圖像之各向異性較低，則可認為2種以上之樹脂相容並形成黏著劑層，或者即便不相容亦均勻分散。另外，於各向異性較高之相位圖像中可觀察到各樹脂呈條紋狀分佈之情況，若相位圖像之各向異性較高，則可認為2種以上之樹脂之混合不均勻。本發明之黏著片材藉由將(P1-avg/P2-avg)設定為上述範圍，可獲得於貼附於半導體晶圓並供於半導體晶圓之背面研磨步驟時可防止研磨水及/或研磨屑滲入至黏著片材與半導體晶圓之間的黏著片材。(P1-avg/P2-avg)較佳為0.97~1.03，更佳為0.98~1.02，進而較佳為0.99~1.01，特別較佳為1。顯示上述範圍之(P1-avg/P2-avg)之黏著劑層例如可藉由適當地選擇構成該黏著劑層之2種以上之樹脂來形成。 The ratio of P 1-avg to P 2-avg (P 1-avg /P 2-avg ) indicates the anisotropy of the phase image. The closer to 1 (P 1-avg /P 2-avg ), the lower the anisotropy; if it is 1, it can be called isotropic. The mixed state of two or more kinds of resins can be estimated from the anisotropy of the phase image. Specifically, when the anisotropy of the phase image is low, it is considered that two or more kinds of resins are compatible and form an adhesive layer, or are uniformly dispersed even if they are incompatible. Further, in the phase image having high anisotropy, it is observed that each resin has a stripe-like distribution, and when the anisotropy of the phase image is high, it is considered that the mixing of two or more kinds of resins is uneven. By setting (P 1-avg /P 2-avg ) to the above range, the adhesive sheet of the present invention can be obtained by preventing the polishing water from sticking to the semiconductor wafer and for the back grinding step of the semiconductor wafer. / or the abrasive chips penetrate into the adhesive sheet between the adhesive sheet and the semiconductor wafer. (P 1-avg /P 2-avg ) is preferably from 0.97 to 1.03, more preferably from 0.98 to 1.02, still more preferably from 0.99 to 1.01, still more preferably 1. The adhesive layer (P 1-avg / P 2-avg ) in the above range can be formed, for example, by appropriately selecting two or more kinds of resins constituting the adhesive layer.
上述P1-avg及P2-avg例如為0.1°~20°。於本發明中，上述P1-avg及P2-avg各自之值的大小對本發明之效果造成之影響較小。無論相位圖像之各方向上之各自的相位差的大小如何，均可藉由調整相位圖像之各向異性(即P1-avg/P2-avg)獲得上述效果，為本發明之成果之一。 The above P 1-avg and P 2-avg are, for example, 0.1° to 20°. In the present invention, the magnitude of each of the above P 1-avg and P 2-avg has little effect on the effect of the present invention. Regardless of the magnitude of the respective phase differences in the respective directions of the phase image, the above effects can be obtained by adjusting the anisotropy of the phase image (ie, P 1-avg /P 2-avg ), which is the result of the present invention. one.
於一個實施形態中，構成黏著劑層之各樹脂分別具有共通之構成單元作為主要構成單元。再者，主要構成單元係指構成各樹脂之構成單元中最多之構成單元。構成黏著劑層之各樹脂中的各樹脂中共通之構成單元的含有比率較佳為40莫耳%以上，更佳為50莫耳%以上，進而較佳為70莫耳%以上，特別較佳為78莫耳%以上。若使用此種具有共通之構成單元之2種以上的樹脂，則樹脂能夠均勻混合而形成上述相位圖像中各向異性較小的樹脂層。 In one embodiment, each of the resins constituting the adhesive layer has a common constituent unit as a main constituent unit. In addition, the main constituent unit means the most constituent unit which comprises the structural unit of each resin. The content ratio of the constituent units common to the respective resins in the respective resins constituting the adhesive layer is preferably 40% by mole or more, more preferably 50% by mole or more, still more preferably 70% by mole or more, and particularly preferably It is 78% or more. When two or more kinds of resins having such a common constituent unit are used, the resin can be uniformly mixed to form a resin layer having less anisotropy in the phase image.
於一個實施形態中，構成黏著劑層之各樹脂間之SP值之差較佳為0(cal/cm3)1/2~2.0(cal/cm3)1/2，更佳為0(cal/cm3)1/2~1.0(cal/cm3)1/2，進而較佳為0(cal/cm3)1/2~0.5(cal/cm3)1/2。若為此種範圍，則樹脂能夠均勻混合而形成上述相位圖像中各向異性較小之樹脂層。 In one embodiment, the difference in SP value between the resins constituting the adhesive layer is preferably 0 (cal/cm 3 ) 1/2 to 2.0 (cal/cm 3 ) 1/2 , more preferably 0 (cal). /cm 3 ) 1/2 to 1.0 (cal/cm 3 ) 1/2 , further preferably 0 (cal/cm 3 ) 1/2 to 0.5 (cal/cm 3 ) 1/2 . When it is such a range, the resin can be uniformly mixed to form a resin layer having a small anisotropy in the above phase image.
於一個實施形態中，構成黏著劑層之各樹脂間之190℃、2.16kgf下的熔融流動速率之差較佳為0g/10min~50g/10min，更佳為0g/10min~20g/10min，進而較佳為0g/10min~15g/10min。若為此種範圍，則樹脂能夠均勻混合而形成上述相位圖像中各向異性較小之樹脂層。熔融流動速率可利用以JIS K 7210為基準之方法來測定。 In one embodiment, the difference in melt flow rate between 190 ° C and 2.16 kgf between the resins constituting the adhesive layer is preferably from 0 g/10 min to 50 g/10 min, more preferably from 0 g/10 min to 20 g/10 min. It is preferably from 0 g/10 min to 15 g/10 min. When it is such a range, the resin can be uniformly mixed to form a resin layer having a small anisotropy in the above phase image. The melt flow rate can be measured by a method based on JIS K 7210.
於本發明中，較佳為如上所述地組合使用黏著性樹脂與非黏著性樹脂作為2種以上之樹脂。於本發明中，藉由具備抑制非黏著性樹脂呈條紋狀分佈之樹脂層，能夠獲得於貼附於半導體晶圓並供於半導體晶圓之背面研磨步驟之情形時，可防止研磨水及/或研磨屑滲入至黏著片材與半導體晶圓之間的黏著片材。 In the present invention, it is preferred to use an adhesive resin and a non-adhesive resin as two or more kinds of resins in combination as described above. In the present invention, by providing a resin layer which suppresses the stripe-like distribution of the non-adhesive resin, it is possible to obtain the polishing water and/or when it is attached to the semiconductor wafer and applied to the back surface polishing step of the semiconductor wafer. Or the abrasive chips penetrate into the adhesive sheet between the adhesive sheet and the semiconductor wafer.
作為上述黏著性樹脂，可使用任意適當之樹脂。作為上述黏著性樹脂，例如可列舉聚烯烴系樹脂、丙烯酸系樹脂、苯乙烯系樹脂等熱塑性樹脂。較佳為使用聚烯烴系樹脂。作為聚烯烴系樹脂之具體例，可列舉低密度聚乙烯、超低密度聚乙烯、非晶質聚丙烯系樹脂(例如，非晶質丙烯-(1-丁烯)共聚物、非晶質丙烯-乙烯共聚物等)、離聚物樹脂、乙烯-乙酸乙烯酯共聚物、乙烯-(甲基)丙烯酸共聚物、乙烯-(甲基)丙烯酸酯-馬來酸酐共聚物、乙烯-甲基丙烯酸縮水甘油酯共聚物等乙烯共聚物、或聚烯烴改性聚合物等。其中較佳為非晶質聚丙烯系樹脂。 As the above adhesive resin, any appropriate resin can be used. Examples of the above-mentioned adhesive resin include thermoplastic resins such as a polyolefin resin, an acrylic resin, and a styrene resin. It is preferred to use a polyolefin resin. Specific examples of the polyolefin resin include low density polyethylene, ultra low density polyethylene, and amorphous polypropylene resin (for example, amorphous propylene-(1-butene) copolymer, amorphous propylene. -ethylene copolymer, etc.), ionomer resin, ethylene-vinyl acetate copolymer, ethylene-(meth)acrylic acid copolymer, ethylene-(meth)acrylate-maleic anhydride copolymer, ethylene-methacrylic acid An ethylene copolymer such as a glycidyl ester copolymer or a polyolefin-modified polymer. Among them, an amorphous polypropylene resin is preferred.
上述黏著性樹脂之230℃、2.16kgf下之熔融流動速率較佳為1g/10min~50g/10min，進而較佳為5g/10min~30g/10min，特別較佳為5g/10min~20g/10min。 The melt flow rate at 230 ° C and 2.16 kgf of the above adhesive resin is preferably from 1 g/10 min to 50 g/10 min, more preferably from 5 g/10 min to 30 g/10 min, particularly preferably from 5 g/10 min to 20 g/10 min.
上述非晶質聚丙烯系樹脂較佳為能夠藉由使用茂金屬觸媒將丙烯與烯烴(例如1-丁烯、乙烯等)聚合而獲得。使用茂金屬觸媒進行聚合獲得之非晶質聚丙烯系樹脂顯示狹窄之分子量分佈。具體而言，上述非晶質聚丙烯系樹脂之分子量分佈(Mw/Mn)為2.5以下，較佳為1.0~2.3，進而較佳為1.0~2.1。分子量分佈狹窄之非晶質聚丙烯系樹脂之低分子量成分較少，因此若使用此種非晶質聚丙烯系樹脂，則能夠獲得可防止由低分子量成分之滲出引起之被黏著體污染之黏著片材。 The amorphous polypropylene-based resin is preferably obtained by polymerizing propylene with an olefin (for example, 1-butene, ethylene, or the like) using a metallocene catalyst. The amorphous polypropylene-based resin obtained by polymerization using a metallocene catalyst exhibits a narrow molecular weight distribution. Specifically, the amorphous polypropylene resin has a molecular weight distribution (Mw/Mn) of 2.5 or less, preferably 1.0 to 2.3, more preferably 1.0 to 2.1. Since the amorphous polypropylene resin having a narrow molecular weight distribution has a small amount of a low molecular weight component, when such an amorphous polypropylene resin is used, it is possible to obtain an adhesion which can be prevented from being contaminated by an adherent due to bleeding of a low molecular weight component. Sheet.
上述非晶質聚丙烯系樹脂中之來自丙烯之構成單元的含有比率較佳為70莫耳%~99莫耳%，進而較佳為75莫耳%~99莫耳%，特別較佳為78莫耳%~99莫耳%。 The content ratio of the constituent unit derived from propylene in the amorphous polypropylene-based resin is preferably from 70 mol% to 99 mol%, more preferably from 75 mol% to 99 mol%, particularly preferably 78. Mole%~99% by mole.
上述非晶質聚丙烯系樹脂中之來自烯烴之構成單元的含有比率較佳為1莫耳%~30莫耳%，進而較佳為1莫耳%~12莫耳%。若為此種範圍，則能夠獲得韌性與柔軟性之平衡優異之黏著片材。 The content ratio of the constituent unit derived from the olefin in the amorphous polypropylene resin is preferably from 1 mol% to 30 mol%, more preferably from 1 mol% to 12 mol%. When it is such a range, the adhesive sheet which is excellent in the balance of toughness and softness can be acquired.
上述非晶質聚丙烯系樹脂可為嵌段共聚物，亦可為無規共聚 物。 The amorphous polypropylene resin may be a block copolymer or a random copolymer Things.
上述非晶質聚丙烯系樹脂之重量平均分子量(Mw)為100,000以上，較佳為100,000~500,000，進而較佳為100,000~300,000。若非晶質聚丙烯系樹脂之重量平均分子量(Mw)為此種範圍，則與一般之苯乙烯系熱塑性樹脂、丙烯酸系熱塑性樹脂(Mw為100,000以下)相比，低分子量成分較少，能夠獲得可防止被黏著體污染之黏著片材。 The amorphous polypropylene resin has a weight average molecular weight (Mw) of 100,000 or more, preferably 100,000 to 500,000, more preferably 100,000 to 300,000. When the weight average molecular weight (Mw) of the amorphous polypropylene resin is in such a range, the amount of the low molecular weight component is smaller than that of a general styrene thermoplastic resin or an acrylic thermoplastic resin (Mw is 100,000 or less). Adhesive sheet that prevents contamination by adherends.
上述非晶質聚丙烯系樹脂於無損本發明之效果之範圍內，亦可進而包含來自其他單體之構成單元。作為其他單體，例如可列舉1-戊烯、1-己烯、1-辛烯、1-癸烯、4-甲基-1-戊烯、3-甲基-1-戊烯等α-烯烴。 The amorphous polypropylene-based resin may further contain constituent units derived from other monomers within the range in which the effects of the present invention are not impaired. Examples of the other monomer include α-pentene, 1-hexene, 1-octene, 1-decene, 4-methyl-1-pentene, and 3-methyl-1-pentene. Olefins.
作為上述非黏著性樹脂，只要與上述黏著性樹脂的混合性良好且不顯示黏著性，則能夠使用任意適當之樹脂。 As the non-adhesive resin, any suitable resin can be used as long as it has good miscibility with the above-mentioned adhesive resin and does not exhibit adhesiveness.
作為能夠與上述非晶質聚丙烯系樹脂組合使用之非黏著性樹脂，例如可列舉乙烯-乙酸乙烯酯共聚物、乙烯-甲基丙烯酸甲酯共聚物、聚酯系樹脂(聚對苯二甲酸乙二酯、聚萘二甲酸乙二酯、聚對苯二甲酸丁二酯、聚萘二甲酸丁二酯等)、聚烯烴系樹脂(聚乙烯、聚丙烯、乙烯-丙烯共聚物等)、聚乙烯醇、聚偏二氯乙烯、聚氯乙烯、氯乙烯-乙酸乙烯酯共聚物、聚乙酸乙烯酯、聚醯胺、聚醯亞胺、纖維素類、氟系樹脂、聚醚、聚苯乙烯系樹脂(聚苯乙烯等)、聚碳酸酯、聚醚碸等。其中，較佳為聚丙烯系樹脂，更佳為結晶性聚丙烯系樹脂。 Examples of the non-adhesive resin that can be used in combination with the amorphous polypropylene-based resin include an ethylene-vinyl acetate copolymer, an ethylene-methyl methacrylate copolymer, and a polyester resin (polyterephthalic acid). Ethylene glycol, polyethylene naphthalate, polybutylene terephthalate, polybutylene naphthalate, etc., polyolefin resin (polyethylene, polypropylene, ethylene-propylene copolymer, etc.), Polyvinyl alcohol, polyvinylidene chloride, polyvinyl chloride, vinyl chloride-vinyl acetate copolymer, polyvinyl acetate, polyamide, polyimine, cellulose, fluorine resin, polyether, polystyrene A vinyl resin (polystyrene or the like), a polycarbonate, a polyether oxime or the like. Among them, a polypropylene resin is preferable, and a crystalline polypropylene resin is more preferable.
上述非黏著性樹脂之230℃、2.16kgf下之熔融流動速率較佳為1g/10min~50g/10min，進而較佳為5g/10min~30g/10min，特別較佳為5g/10min~20g/10min。 The melt flow rate at 230 ° C and 2.16 kgf of the non-adhesive resin is preferably from 1 g/10 min to 50 g/10 min, further preferably from 5 g/10 min to 30 g/10 min, particularly preferably from 5 g/10 min to 20 g/10 min. .
上述聚丙烯系樹脂可為均聚物，亦可為以來自丙烯之構成單元為主要構成單元之共聚物。該共聚物包含來自例如乙烯、1-戊烯、1- 己烯、1-辛烯、1-癸烯、4-甲基-1-戊烯、α-烯烴等能夠與丙烯共聚之單體的構成單元。上述聚丙烯系樹脂較佳為與上述非晶質聚丙烯系樹脂同樣，可藉由使用茂金屬觸媒進行聚合來獲得。 The polypropylene resin may be a homopolymer or a copolymer having a constituent unit derived from propylene as a main constituent unit. The copolymer comprises, for example, ethylene, 1-pentene, 1- A constituent unit of a monomer copolymerizable with propylene such as hexene, 1-octene, 1-decene, 4-methyl-1-pentene or α-olefin. The polypropylene resin is preferably obtained by polymerization using a metallocene catalyst, similarly to the above amorphous polypropylene resin.
上述黏著性樹脂與非黏著性樹脂之混合比率可根據所期望之黏著力設為任意適當之混合比率。例如，組合使用非晶質聚丙烯系樹脂與結晶性聚丙烯系樹脂之情形時，結晶性聚丙烯系樹脂之含有比率較佳為相對於上述非晶質聚丙烯系樹脂與該結晶性聚丙烯系樹脂之合計重量，較佳為50重量%以下，進而較佳為40重量%以下，特別較佳為30重量%以下。 The mixing ratio of the above adhesive resin to the non-adhesive resin can be set to any appropriate mixing ratio according to the desired adhesive force. For example, when an amorphous polypropylene resin and a crystalline polypropylene resin are used in combination, the content ratio of the crystalline polypropylene resin is preferably relative to the amorphous polypropylene resin and the crystalline polypropylene. The total weight of the resin is preferably 50% by weight or less, more preferably 40% by weight or less, and particularly preferably 30% by weight or less.
上述黏著劑層於無損本發明之效果之範圍內可進而包含其他成分。作為該其他成分，例如可列舉抗氧化劑、紫外線吸收劑、光穩定劑、耐熱穩定劑、抗靜電劑等。其他成分之種類及使用量可根據目的適當選擇。 The above-mentioned adhesive layer may further contain other components within the range which does not impair the effects of the present invention. Examples of the other component include an antioxidant, an ultraviolet absorber, a light stabilizer, a heat stabilizer, an antistatic agent, and the like. The types and amounts of other ingredients may be appropriately selected depending on the purpose.
黏著劑層10之厚度較佳為5μm~100μm，進而較佳為10μm~65μm。 The thickness of the adhesive layer 10 is preferably 5 μm to 100 μm, and more preferably 10 μm to 65 μm.
B.其他層 B. Other layers
本發明之黏著片材除上述黏著劑層以外，亦可進而具備任意適當之其他層。 The adhesive sheet of the present invention may further comprise any other suitable layer in addition to the above-mentioned adhesive layer.
圖2係本發明之一個實施形態之黏著片材之概略剖面圖。黏著片材100依次具備黏著劑層10、中間層20、及基材層20。 Fig. 2 is a schematic cross-sectional view showing an adhesive sheet according to an embodiment of the present invention. The adhesive sheet 100 includes the adhesive layer 10, the intermediate layer 20, and the base material layer 20 in this order.
黏著片材100之厚度較佳為90μm~300μm，更佳為100μm~260μm。 The thickness of the adhesive sheet 100 is preferably from 90 μm to 300 μm, more preferably from 100 μm to 260 μm.
中間層20之厚度較佳為50μm~200μm，更佳為80μm~180μm。 The thickness of the intermediate layer 20 is preferably from 50 μm to 200 μm, more preferably from 80 μm to 180 μm.
中間層20可由任意適當之樹脂構成。作為構成中間層20之樹脂，較佳使用能夠擠出成形之樹脂，更佳使用能夠與構成黏著劑層之樹脂及構成基材層之樹脂共擠出成形的樹脂。作為構成中間層20之樹 脂之具體例，可列舉乙烯-乙酸乙烯酯共聚物、乙烯-甲基丙烯酸甲酯共聚物、聚酯系樹脂(聚對苯二甲酸乙二酯、聚萘二甲酸乙二酯、聚對苯二甲酸丁二酯、聚萘二甲酸丁二酯等)、聚烯烴系樹脂(聚乙烯、聚丙烯、乙烯-丙烯共聚物等)、聚乙烯醇、聚偏二氯乙烯、聚氯乙烯、氯乙烯-乙酸乙烯酯共聚物、聚乙酸乙烯酯、聚醯胺、聚醯亞胺、纖維素類、氟系樹脂、聚醚、聚苯乙烯系樹脂(聚苯乙烯等)、聚碳酸酯、聚醚碸等。 The intermediate layer 20 can be composed of any suitable resin. As the resin constituting the intermediate layer 20, a resin which can be extrusion-molded is preferably used, and a resin which can be co-extruded with a resin constituting the pressure-sensitive adhesive layer and a resin constituting the substrate layer is more preferably used. As the tree constituting the intermediate layer 20 Specific examples of the fat include an ethylene-vinyl acetate copolymer, an ethylene-methyl methacrylate copolymer, and a polyester resin (polyethylene terephthalate, polyethylene naphthalate, polyparaphenylene) Polybutylene dicarboxylate, polybutylene naphthalate, etc.), polyolefin resin (polyethylene, polypropylene, ethylene-propylene copolymer, etc.), polyvinyl alcohol, polyvinylidene chloride, polyvinyl chloride, chlorine Ethylene-vinyl acetate copolymer, polyvinyl acetate, polyamide, polyimine, cellulose, fluorine resin, polyether, polystyrene resin (polystyrene, etc.), polycarbonate, poly Ether oxime and the like.
構成中間層20之樹脂之190℃、2.16kgf下的熔融流動速率較佳為2g/10min~20g/10min，進而較佳為5g/10min~15g/10min，特別較佳為7g/10min~12g/10min。若為此種範圍，則能夠藉由共擠出成形而無加工不良地形成中間層。 The melt flow rate at 190 ° C and 2.16 kgf of the resin constituting the intermediate layer 20 is preferably from 2 g/10 min to 20 g/10 min, more preferably from 5 g/10 min to 15 g/10 min, particularly preferably from 7 g/10 min to 12 g/ 10min. If it is such a range, an intermediate layer can be formed by co-extrusion molding without a process defect.
基材層30之厚度較佳為10μm~200μm，更佳為20μm~150μm。 The thickness of the base material layer 30 is preferably from 10 μm to 200 μm, more preferably from 20 μm to 150 μm.
基材層30可由任意適當之樹脂構成。作為構成基材層30之樹脂，較佳使用能夠擠出成形之樹脂，更佳使用能夠與構成黏著劑層之樹脂及構成中間層之樹脂共擠出成形的樹脂。作為構成基材層30之樹脂之具體例，可列舉乙烯-乙酸乙烯酯共聚物、乙烯-甲基丙烯酸甲酯共聚物、聚酯系樹脂(聚對苯二甲酸乙二酯、聚萘二甲酸乙二酯、聚對苯二甲酸丁二酯、聚萘二甲酸丁二酯等)、聚烯烴系樹脂(聚乙烯、聚丙烯、乙烯-丙烯共聚物等)、聚乙烯醇、聚偏二氯乙烯、聚氯乙烯、氯乙烯-乙酸乙烯酯共聚物、聚乙酸乙烯酯、聚醯胺、聚醯亞胺、纖維素類、氟系樹脂、聚醚、聚苯乙烯系樹脂(聚苯乙烯等)、聚碳酸酯、聚醚碸等。 The base material layer 30 may be composed of any suitable resin. As the resin constituting the base material layer 30, a resin which can be extrusion-molded is preferably used, and a resin which can be co-extruded with a resin constituting the pressure-sensitive adhesive layer and a resin constituting the intermediate layer is more preferably used. Specific examples of the resin constituting the base material layer 30 include an ethylene-vinyl acetate copolymer, an ethylene-methyl methacrylate copolymer, and a polyester resin (polyethylene terephthalate, polyethylene naphthalate). Ethylene glycol ester, polybutylene terephthalate, polybutylene naphthalate, etc.), polyolefin resin (polyethylene, polypropylene, ethylene-propylene copolymer, etc.), polyvinyl alcohol, polyvinylidene chloride Ethylene, polyvinyl chloride, vinyl chloride-vinyl acetate copolymer, polyvinyl acetate, polyamide, polyimine, cellulose, fluorine resin, polyether, polystyrene resin (polystyrene, etc.) ), polycarbonate, polyether oxime, etc.
基材層30之230℃、2.16kgf下之熔融流動速率較佳為1g/10min~50g/10min，進而較佳為5g/10min~30g/10min，特別較佳為5g/10min~25g/10min。 The melt flow rate at 230 ° C and 2.16 kgf of the base material layer 30 is preferably from 1 g/10 min to 50 g/10 min, further preferably from 5 g/10 min to 30 g/10 min, particularly preferably from 5 g/10 min to 25 g/10 min.
中間層20及基材層30於無損本發明之效果之範圍內亦可進而包 含其他成分。作為該其他成分，例如可使用與上述A項中所說明之黏著劑層中可包含之其他成分相同的成分。 The intermediate layer 20 and the substrate layer 30 may further include a range that does not impair the effects of the present invention. Contains other ingredients. As the other component, for example, the same components as those other components which can be contained in the adhesive layer described in the above item A can be used.
本發明之黏著片材根據需要亦可進而具備其他層。例如，本發明之黏著片材亦可進而具備在供於實用之前保護黏著劑層的保護層。本發明之黏著片材於被保護層保護之狀態下可捲取為輥狀。作為保護層，例如可列舉利用矽系剝離劑、氟系剝離劑、長鏈丙烯酸烷基酯系剝離劑等剝離劑進行表面塗佈之塑膠(例如，聚對苯二甲酸乙二酯(PET)、聚乙烯、聚丙烯)薄膜、不織布或紙等。 The adhesive sheet of the present invention may further have other layers as needed. For example, the adhesive sheet of the present invention may further have a protective layer that protects the adhesive layer before being supplied for practical use. The adhesive sheet of the present invention can be wound into a roll shape in a state protected by a protective layer. Examples of the protective layer include a surface-coated plastic (for example, polyethylene terephthalate (PET)) using a release agent such as a ruthenium release agent, a fluorine release agent, or a long-chain alkyl acrylate release agent. , polyethylene, polypropylene) film, non-woven fabric or paper.
本發明之黏著片材例如於未用保護層保護之情形時，亦可於與黏著劑層相反側之最外層進行背面處理。背面處理可使用例如矽系剝離劑或長鏈丙烯酸烷基酯系剝離劑等剝離劑來進行。本發明之黏著片材藉由進行背面處理，可捲取為輥狀。 The adhesive sheet of the present invention may be subjected to a back treatment on the outermost side opposite to the adhesive layer, for example, when it is not protected by a protective layer. The back surface treatment can be carried out using, for example, a release agent such as a ruthenium release agent or a long-chain alkyl acrylate release agent. The adhesive sheet of the present invention can be wound into a roll shape by performing back treatment.
C.黏著片材之製造方法 C. Method for manufacturing adhesive sheet
本發明之黏著片材較佳為將構成黏著片材之各層(例如，黏著劑層、中間層、基材層)之形成材料共擠出成形而製造。藉由共擠出成形，能夠以較少之步驟數且不使用有機溶劑而製造層間之接著性良好的黏著片材。 The adhesive sheet of the present invention is preferably produced by co-extruding a material for forming the respective layers (for example, an adhesive layer, an intermediate layer, and a substrate layer) constituting the adhesive sheet. By co-extrusion molding, it is possible to produce an adhesive sheet having good adhesion between layers with a small number of steps and without using an organic solvent.
上述共擠出成形中，構成黏著片材之各層之形成材料可使用藉由任意適當之方法將各層之成分混合而成的材料。黏著劑層之形成材料較佳為將構成該黏著劑層之2種以上之樹脂熔融並混合。作為構成黏著劑層之2種以上之樹脂的混合方法，例如可列舉：自單一料斗向擠出機供給將樹脂顆粒彼此於顆粒狀態下摻合的混合物，並於熔融擠出成形時使其混合的方法；將樹脂顆粒自2個以上之料斗控制各自流量向擠出機進行供給，並於熔融擠出成形時使其混合的方法；事先用混練機等將樹脂顆粒彼此摻合製作母料，自單一料斗向擠出機進行供給，並於熔融擠出成形時使其混合的方法等。 In the above coextrusion molding, a material constituting each layer of the adhesive sheet may be a material obtained by mixing the components of the respective layers by any appropriate method. The material for forming the pressure-sensitive adhesive layer is preferably such that two or more kinds of resins constituting the pressure-sensitive adhesive layer are melted and mixed. As a method of mixing the two or more kinds of resins constituting the pressure-sensitive adhesive layer, for example, a mixture in which resin particles are blended in a granular state is supplied from a single hopper to an extruder, and is mixed at the time of melt extrusion molding. a method of supplying resin pellets to two or more hoppers to control respective flow rates to an extruder, and mixing them during melt extrusion molding; premixing resin pellets with each other by a kneading machine or the like to prepare a master batch, A method in which a single hopper is supplied to an extruder and mixed at the time of melt extrusion molding.
作為上述共擠出成形之具體方法，例如可列舉：對連接有模嘴之複數個擠出機分別供給構成黏著片材之各層之形成材料，熔融後擠出，利用接觸輥成形法收取，並將積層體成形的方法。 As a specific method of the above-described co-extrusion molding, for example, a material for forming each layer constituting the adhesive sheet is supplied to a plurality of extruders to which a die is connected, melted, extruded, and charged by a contact roll forming method. A method of forming a laminate.
上述共擠出成形中之成形溫度較佳為160℃~220℃，進而較佳為170℃~200℃。若為此種範圍，則成形穩定性優異。 The molding temperature in the above coextrusion molding is preferably from 160 ° C to 220 ° C, more preferably from 170 ° C to 200 ° C. When it is such a range, it is excellent in shaping|molding stability.
上述共擠出成形中之製膜速度較佳為3m/min~30m/min。 The film forming speed in the above coextrusion molding is preferably from 3 m/min to 30 m/min.
上述共擠出成形中之接觸輥之溫度較佳為15℃~80℃。 The temperature of the contact roll in the above coextrusion molding is preferably from 15 ° C to 80 ° C.
以下，藉由實施例具體說明本發明，但本發明不受該等實施例之任何限定。再者，份表示重量份。 Hereinafter, the present invention will be specifically described by way of examples, but the present invention is not limited by the examples. Further, parts represent parts by weight.
作為黏著劑層形成材料，使用利用茂金屬觸媒進行聚合之非晶質丙烯-(1-丁烯)共聚物(住友化學公司製造，商品名「TAFTHREN H5002」、來自丙烯之構成單元90莫耳%/來自1-丁烯之構成單元10莫耳%、Mw=230,000、Mw/Mn=1.8)80份及利用茂金屬觸媒進行聚合之丙烯-乙烯共聚物(日本聚丙烯公司製造，商品名「WINTEC WFX4」、來自丙烯之構成單元96莫耳%/來自乙烯之構成單元4莫耳%、熔點：125℃、軟化點115℃)20份的混合物。非晶質丙烯-(1-丁烯)共聚物與聚丙烯-乙烯共聚物之混合係藉由自單一料斗向擠出機供給將樹脂顆粒彼此於顆粒狀態下摻合的混合物，並於熔融擠出成形時使其混合的方法來進行。 As the adhesive layer forming material, an amorphous propylene-(1-butene) copolymer polymerized by a metallocene catalyst (manufactured by Sumitomo Chemical Co., Ltd., trade name "TAFTHREN H5002", and a constituent unit derived from propylene 90 mol are used. %/80 parts of constituent units derived from 1-butene, Mw=230,000, Mw/Mn=1.8) 80 parts and propylene-ethylene copolymer polymerized by metallocene catalyst (manufactured by Nippon Polypropylene Co., Ltd., trade name A mixture of "WINTEC WFX4", a constituent unit derived from propylene 96 mol% / a constituent unit derived from ethylene 4 mol%, a melting point: 125 ° C, and a softening point of 115 ° C). The mixture of the amorphous propylene-(1-butene) copolymer and the polypropylene-ethylene copolymer is supplied to the extruder from a single hopper to a mixture of the resin particles in a particulate state, and is melt extruded. A method of mixing them during molding is carried out.
作為中間層形成材料，使用乙烯-乙酸乙烯酯共聚物(三井杜邦公司製造，商品名「V523」)。 As the intermediate layer forming material, an ethylene-vinyl acetate copolymer (manufactured by Mitsui DuPont, trade name "V523") was used.
作為基材層形成材料，使用利用茂金屬觸媒進行聚合之聚丙烯-乙烯共聚物(日本聚丙烯公司製造，商品名「WINTFC WSX02」)。 As the base layer forming material, a polypropylene-ethylene copolymer (manufactured by Nippon Polypropylene Co., Ltd., trade name "WINTFC WSX02") which is polymerized by a metallocene catalyst is used.
將上述黏著劑形成材料、中間層形成材料及基材層形成材料進 行T模嘴熔融共擠出(擠出溫度：180℃、製膜速度：5m/min)，將熔融狀態之樹脂與向接觸輥成形部(接觸輥溫度：50℃)通紙之塗佈有Si的PET隔膜(帝人杜邦公司製造，商品名「Tetoron Film G2」)積層後，進行冷卻，獲得黏著片材(基材層(厚度：30μm)/中間層(厚度：90μm)/黏著劑層(厚度：10μm)/保護層(厚度：50μm))。 The above-mentioned adhesive forming material, intermediate layer forming material, and base material forming material are The T-die melt co-extrusion (extrusion temperature: 180 ° C, film forming speed: 5 m / min), and the molten resin and the contact roll forming portion (contact roll temperature: 50 ° C) were coated with paper. Si PET film (manufactured by Teijin DuPont, trade name "Tetoron Film G2") was laminated, and then cooled to obtain an adhesive sheet (base material layer (thickness: 30 μm) / intermediate layer (thickness: 90 μm) / adhesive layer ( Thickness: 10 μm) / protective layer (thickness: 50 μm)).
將構成樹脂層之樹脂、構成中間層之樹脂、共擠出成形中之製膜速度、以及共擠出成形中之接觸輥溫度設定為如表1所示，除此以外，以與實施例1同樣之方式，獲得黏著片材。 The resin constituting the resin layer, the resin constituting the intermediate layer, the film forming speed in the coextrusion molding, and the contact roll temperature in the coextrusion molding were set as shown in Table 1, and the same as Example 1 In the same way, an adhesive sheet is obtained.
再者，表1中記載之樹脂之詳細情況如下所述。 In addition, the details of the resin described in Table 1 are as follows.
「WK307」：乙烯-甲基丙烯酸甲酯共聚物(住友化學公司製造，商品名「WK307」) "WK307": Ethylene-methyl methacrylate copolymer (manufactured by Sumitomo Chemical Co., Ltd., trade name "WK307")
「H6822S」：包含丙烯-(1-丁烯)共聚物、苯乙烯系聚合物、乙烯系聚合物與丁二烯系聚合物的樹脂混合物(住友化學公司製造，商品名「TAFTHREN H6822S」) "H6822S": a resin mixture containing a propylene-(1-butene) copolymer, a styrene-based polymer, a vinyl polymer, and a butadiene-based polymer (manufactured by Sumitomo Chemical Co., Ltd., trade name "TAFTHREN H6822S")
「Vistamaxx 6202」：非晶質丙烯-乙烯共聚物(ExxonMobil Chemical公司製造，商品名「Vistamaxx 6202」，來自丙烯之構成單元78莫耳%/來自乙烯之構成單元22莫耳%、MFR(230℃、2.16kgf)=18g/10min、分子量分佈：Mw/Mn=2.05、Tg=-31.8℃) "Vistamaxx 6202": amorphous propylene-ethylene copolymer (manufactured by ExxonMobil Chemical Co., Ltd., trade name "Vistamaxx 6202", constituent unit derived from propylene 78 mol% / constituent unit derived from ethylene 22 mol%, MFR (230 ° C , 2.16kgf) = 18g/10min, molecular weight distribution: Mw / Mn = 2.05, Tg = -31.8 ° C)
「FLX80E4」：均聚聚丙烯(住友化學公司製造，商品名「FLX80E4」) "FLX80E4": homopolypropylene (manufactured by Sumitomo Chemical Co., Ltd., trade name "FLX80E4")
「WMG03」：丙烯-乙烯共聚物(日本聚丙烯公司製造，商品名「WINTEC WMG03」，來自丙烯之構成單元99莫耳%/來自乙烯之構成單元1莫耳%、熔點：142℃、軟化點：130℃) "WMG03": propylene-ethylene copolymer (manufactured by Nippon Polypropylene Co., Ltd., trade name "WINTEC WMG03", constituent unit derived from propylene 99 mol% / constituent unit derived from ethylene 1 mol%, melting point: 142 ° C, softening point :130°C)
「Vistamaxx 3980FL」：丙烯-乙烯共聚物(ExxonMobil Chemical公司製造，商品名「Vistamaxx 3980FL」，來自丙烯之構成單元87莫 耳%/來自乙烯之構成單元13莫耳%、MFR：8g/10min，分子量分布)[評價] "Vistamaxx 3980FL": propylene-ethylene copolymer (manufactured by ExxonMobil Chemical Co., Ltd., trade name "Vistamaxx 3980FL", from the constituent unit of propylene 87 Ear % / constituent unit derived from ethylene 13 mol%, MFR: 8 g/10 min, molecular weight distribution) [Evaluation]
將實施例及比較例中獲得之黏著片材供於以下評價。結果示於表1。 The adhesive sheets obtained in the examples and the comparative examples were subjected to the following evaluations. The results are shown in Table 1.
(1)黏著劑層之各向異性 (1) Anisotropy of the adhesive layer
自實施例及比較例中獲得之黏著片材剝離保護層(塗佈有Si之PET隔膜)，利用原子力顯微鏡(Veeco公司製造，NanoScope-3D)測定黏著劑層之露出面之相位圖像。作為原子力顯微鏡之懸臂，使用輕敲模式用之單晶矽製造、懸臂長為160μm、力接觸(force contact)為26N/m、共振頻率為200~400kHz之懸臂(Olympus公司製造，OMLC-AC160TS-C3)。測定係於室溫23℃、輕敲模式下進行。以256pixel×256pixel掃描5μm×5μm之範圍，掃描速度設為0.5~1.0Hz。 The adhesive sheet peeling protective layer (PET film coated with Si) obtained in the examples and the comparative examples was measured for the phase image of the exposed surface of the adhesive layer by an atomic force microscope (manufactured by Veeco, Inc., NanoScope-3D). As a cantilever of the atomic force microscope, it is manufactured by a single crystal crucible using a tapping mode, a cantilever length of 160 μm, a force contact of 26 N/m, and a resonance frequency of 200 to 400 kHz (Olympus, OMLC-AC160TS- C3). The measurement was carried out at room temperature of 23 ° C in a tapping mode. The range of 5 μm × 5 μm is scanned by 256 pixels × 256 pixels, and the scanning speed is set to 0.5 to 1.0 Hz.
將如上所述測定而獲得之相位圖像用圖像分析軟體進行處理，評價黏著劑層之各向異性。具體而言，按照以下順序評價黏著劑層之各向異性。 The phase image obtained as described above was processed by an image analysis software to evaluate the anisotropy of the adhesive layer. Specifically, the anisotropy of the adhesive layer was evaluated in the following order.
對獲得之相位圖像進行傾斜校正後，取得以縱軸(y軸)為相位差(基於原子力顯微鏡測定之輸入信號與輸出信號之相位差(°))、以橫軸(x軸)為測定距離之第1方向(寬度方向(TD))及第2方向(長度方向(MD))的線分佈，根據上述式(1)求出各方向上之相位差之大小P1、P2。分別於各方向上求出隨機提取之128條線之P1、P2，計算其平均P1-avg、P2-avg，根據(P1-avg/P2-avg)評價黏著劑層之各向異性。 After the obtained phase image is tilt-corrected, the vertical axis (y-axis) is obtained as a phase difference (phase difference (°) between the input signal and the output signal measured by the atomic force microscope), and the horizontal axis (x-axis) is measured. The line distributions of the first direction (width direction (TD)) and the second direction (longitudinal direction (MD)) of the distance are obtained by the above equation (1) by the magnitudes P 1 and P 2 of the phase differences in the respective directions. The P 1 and P 2 of the randomly extracted 128 lines were obtained from the respective directions, and the average P 1-avg and P 2-avg were calculated, and the adhesive layer was evaluated according to (P 1-avg /P 2-avg ). Anisotropy.
(2)水滲入 (2) Water infiltration
自實施例及比較例中獲得之黏著片材剝離保護層後，將該黏著片材貼附於Si鏡面晶圓，將Si鏡面晶圓之背面(與貼附面相反側)研磨至100μm。研磨後，自Si鏡面晶圓剝離黏著片材時，將於黏著片材與Si鏡面晶圓之間確認到水滴的情況設為有水滲入(表1中×)、未確認到 的情況設為無水滲入(表1中○)。 After the adhesive sheet peeling protective layer obtained in the examples and the comparative examples, the adhesive sheet was attached to the Si mirror wafer, and the back surface (the side opposite to the bonding surface) of the Si mirror wafer was polished to 100 μm. When the adhesive sheet was peeled off from the Si mirror wafer after the polishing, water droplets were observed between the adhesive sheet and the Si mirror wafer, and water infiltration (in Table 1) was not confirmed. In the case of no water infiltration (○ in Table 1).
由表1可明確，具備利用原子力顯微鏡之相位圖像之各向異性較小的黏著劑層的本申請案的黏著片材之水滲入較少。 As is clear from Table 1, the adhesive sheet of the present application having the adhesive layer having a small anisotropy of the phase image of the atomic force microscope has less water infiltration.
本發明之黏著片材能夠較佳地用於例如半導體裝置製造時之工件(半導體晶圓等)之暫時固定及保護。 The adhesive sheet of the present invention can be preferably used for temporary fixing and protection of a workpiece (semiconductor wafer or the like) at the time of manufacture of a semiconductor device.
10‧‧‧黏著劑層 10‧‧‧Adhesive layer
20‧‧‧中間層 20‧‧‧Intermediate
30‧‧‧基材層 30‧‧‧Substrate layer
100‧‧‧黏著片材 100‧‧‧Adhesive sheets
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| JP6159163B2 (en) * | 2013-06-21 | 2017-07-05 | 日東電工株式会社 | Adhesive sheet |
| DE102018109269A1 (en) | 2018-04-18 | 2019-10-24 | Clariant Plastics & Coatings Ltd | Permanently tacky pressure-sensitive adhesives with improved environmental compatibility |
| CN113165136B (en) * | 2019-02-26 | 2023-06-13 | 株式会社迪思科 | Adhesive sheet for grinding back surface and method for manufacturing semiconductor wafer |
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| JP2001172453A (en) * | 1999-12-14 | 2001-06-26 | Basell Technology Co Bv | Propylene resin composition |
| JP2001170956A (en) * | 1999-12-17 | 2001-06-26 | Tokuyama Corp | Injection-molded object formed of polypropylene resin |
| EP1502731A1 (en) * | 2003-07-28 | 2005-02-02 | Guy Breger | Composite packaging film and its preparation |
| KR100837013B1 (en) * | 2004-03-19 | 2008-06-10 | 미쯔이카가쿠 가부시기가이샤 | Adhesive material, pressure sensitive adhesive film and method of use thereof |
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| JP5736139B2 (en) * | 2010-09-16 | 2015-06-17 | 日東電工株式会社 | Adhesive tape |
| JP5685118B2 (en) * | 2011-03-17 | 2015-03-18 | 日東電工株式会社 | Adhesive tape |
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