TW200914568A - Resin bleed-out preventing agent and resin bleed-out preventing method - Google Patents

Resin bleed-out preventing agent and resin bleed-out preventing method Download PDF

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Publication number
TW200914568A
TW200914568A TW097116595A TW97116595A TW200914568A TW 200914568 A TW200914568 A TW 200914568A TW 097116595 A TW097116595 A TW 097116595A TW 97116595 A TW97116595 A TW 97116595A TW 200914568 A TW200914568 A TW 200914568A
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TW
Taiwan
Prior art keywords
resin
integer
agent
group
preventing agent
Prior art date
Application number
TW097116595A
Other languages
Chinese (zh)
Other versions
TWI384047B (en
Inventor
Akihiro Aiba
Tomoharu Mimura
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Nippon Mining Co
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Publication date
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Publication of TW200914568A publication Critical patent/TW200914568A/en
Application granted granted Critical
Publication of TWI384047B publication Critical patent/TWI384047B/en

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
    • H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
    • H01L23/293—Organic, e.g. plastic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
    • C09J5/02—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving pretreatment of the surfaces to be joined
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/49—Phosphorus-containing compounds
    • C08K5/51—Phosphorus bound to oxygen
    • C08K5/52—Phosphorus bound to oxygen only
    • C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
    • C09J5/06—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving heating of the applied adhesive
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
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Abstract

An objective of the present invention is to provide a resin bleed-out preventing agent having a low drain-processing load, which do not cause bad effect to die-bonding strength and assembly characteristics and do not impair effects of discoloration preventing processing and sealing processing even in a case that it is used for die-bonding resin of low stress type. The resin bleed-out preventing agent includes a phosphoric acid ester represented by the following formula. O=P(O-(R2-O)n-R1)m(OH)3-m (wherein R1 represents C4 to 30 saturated or unsaturated hydrocarbon group, R2 represents lower alkylene group, n represents an integer of 0 to 10, m represents an integer of 1 to 3.)

Description

200914568 九、發明說明： 【發明所屬之技術領域】 本發明係有關在將引線框架（lead frame)或印刷配線 板等半導體配線基材與1C晶片藉由樹脂而予以接著固定 之黏晶步驟中的樹脂滲出防止劑及防止方法。 【先前技術】 半導體晶片與引線框架或印刷配線板等基材，通常藉 由黏晶樹脂予以接著固定。基材的接著面一般係施以金、3 銀、鈀、銅、鎳等鍍層，惟若表面粗度過大或表面經電鍍 添加劑、變色防止劑、封孔處理劑等有機物污染，則在黏 晶步驟中之黏晶樹脂塗佈時，會產生樹脂或添加劑的滲1 (Resin Bleed 0ut(RB0))。該RB〇係使黏晶強度降低〔並 對作為其後之步驟的打線接合（wire b〇nding)與模封 (moulding)造成不好的影響。 、 則主：為了防止RB〇，係使接著面之電鍍面的表㈣ 管㈣，或洗淨表面以去除污染物。惟 ;之'^面粗度會對黏晶強度、或組裝機深 職hine)之影像辨識能力造成影響，故^ 無差別地減小。此外，在 或封孔處理覆膜也稅離㈣’有連變色防増 材浸題’在專利文獻1中揭示有藉由將基 數分等作為主成分的溶液中並吸附1至 是不合將變“!= 可改變基材面之表面粗度、或 ^色防止覆膜或封孔處理覆膜洗淨_，此外 320190 5 200914568 由於吸附之有機覆膜非常地薄，故不會對打線接合性 封性等組裝特性造成不好的影響，而可防止RB〇。 、 户此外，本發明人等再進行檢討，結果顯示具有極性基 =氟烷化合物係較專利文獻1之羧酸、硫醇化合物等有= 高的RB0防止效果（專利文獻2)。 妒惟，由於說烷化合物含有氟，有排水會造成問題的情 [專利文獻1]曰本特開平^495662號公報 [專利文獻2]日本特願2007-52890號 【發明内容】 (發明欲解決的課題） 本發明之目的在於提供一種樹脂滲出防止劑，其排水 處理之負荷小，且即使在使用低應力型之黏晶樹脂時，也 不會對黏晶強度或組裝特性.造成不好的影響，且不會損及 變色防止處理或封孔處理效果。 、 (解決課題的手段） 4、主本發明人等進行努力研究的結果，發現在藉由將基材 /又/貝於含有樹脂滲出防止劑的溶液並使有機覆膜吸附於電 鍍面之表面而防止樹脂滲出的步驟中，即使在使用排水處 理之負荷較含氟化合物小且較低應力型之黏晶樹脂時，也 I會對黏晶強度或組裝特性造成不好的影響，且不會損及 變色防止處理或封孔處理效果之具有樹脂滲出防止效果的 群有機化合物，而完成本發明。 亦即’本發明係如以下敘述。 6 320190 200914568 (1)一種樹脂滲出防止劑，包含以下述通式表示之磷酸 酉旨 〇=P(〇-(R2-0)n-R1)m(〇H)3 m (式中，R!為碳數4至30的飽和或不飽和之烴基，R2為低 級伸院基，η為0至1〇的整數，①為1至3的整數）。 (2)如上述（1)記载之樹脂滲出防止劑，其中，上述磷酸 酯之Κ為碳數8至20的烷基、烯基、炔基之任一者，R2 為伸乙基’η為1至6的整數，j至3的整數。 _ (3)如上述（1)或（2)記載之樹腊滲出防止劑，復包含： 含有四唾衍生物、三唾衍生物、味峻衍生物、嗟唾衍生物 之任一者的含氮雜環狀化合物系變色防止劑。 一 W-種樹月旨渗出防止方法，係使用上述⑴至（3)中任 一項記^之樹脂滲出防止劑施以樹脂渗出防止處理。 樹月Λ5)Φ—種基材❹上述⑴至⑺中任—項記載之 防止劑施《樹轉出防止處理，而具有 出防止劑之覆膜。 (發明的效果） 印刷配本發明之樹脂渗出防止劑進行在引線框架、 止功能乏二：：體配線基材的表面吸附具有樹脂滲出防 防止效果或卢物的樹月旨渗出防止處理，可不損及變色 出。此外Γ理效果而防止在黏晶步驟中之樹月旨滲 不好的影響。更線接合性或模封性等組襄特性造成 處理之負荷小。為非氣系之樹脂滲出防止劑，故排水 320190 7 200914568 *【實施方式】 , 本發明之樹脂滲出防止劑包含以下述通式表示之磷酸 酯： 〇=P(〇-(R2-0)n-R1)m(〇H)3.m (式中，R!為碳數4至30的飽和或不飽和之烴基，R2為低 級伸烷基，η為〇至1〇的整數，瓜為1至3的整數）。[Technical Field] The present invention relates to a die bonding step in which a semiconductor wiring substrate such as a lead frame or a printed wiring board and a 1C wafer are subsequently fixed by a resin. Resin exudation preventing agent and prevention method. [Prior Art] A substrate such as a semiconductor wafer and a lead frame or a printed wiring board is usually fixed by a die bonding resin. The adhesion surface of the substrate is generally applied with gold, 3 silver, palladium, copper, nickel, etc., but if the surface roughness is too large or the surface is contaminated by organic substances such as plating additives, discoloration inhibitors, sealing treatment agents, etc., In the step of coating the die-casting resin, a resin or additive is formed (Resin Bleed 0ut (RB0)). The RB lanthanum reduces the strength of the die bond [and causes a bad influence on wire b〇nding and molding as a subsequent step. Then, in order to prevent RB 〇, the surface (4) of the plating surface of the bonding surface is used, or the surface is cleaned to remove contaminants. However, the '^ surface roughness affects the image identification ability of the die bond strength or the assembly machine's deep hine, so it is reduced indiscriminately. In addition, the film is also taxed or sealed (4) 'There is a color-changing anti-crust material immersion problem'. Patent Document 1 discloses that a solution having a base component is used as a main component and adsorbs 1 to be inconsistent. "!= Can change the surface roughness of the substrate surface, or color to prevent filming or sealing treatment of the film to wash _, in addition, 320190 5 200914568 Because the organic film adsorbed is very thin, it will not be wire bonding In addition, the inventors of the present invention conducted a review, and the results showed that the polar group = fluoroalkane compound is a carboxylic acid or a thiol compound of Patent Document 1 because it has a bad influence on the assembly property such as the sealing property. In the case of the arsenal of the arsenal of the arsenal of the arsenal of the arsenal of the arsenal of the arsenal of the arsenal of the arsenal of the arsenal Japanese Patent Application No. 2007-52890 (Problem to be Solved by the Invention) An object of the present invention is to provide a resin bleed prevention agent which has a small load for drainage treatment and which is used even when a low-stress type varnish resin is used. Will not stick to the crystal Intensity or assembly characteristics. It does not affect the effect of discoloration prevention or sealing treatment. (The means to solve the problem) 4. The results of the intensive study by the inventor, etc. In the step of preventing the resin from oozing out from the substrate/again/the solution containing the resin bleed prevention agent and adsorbing the organic film on the surface of the plating surface, even if the load using the drainage treatment is smaller than the fluorine-containing compound and the lower stress type In the case of the die-bonding resin, the group I organic compound which has a bad influence on the die strength or the assembly property and which does not impair the effect of the discoloration prevention treatment or the sealing treatment effect, and which has the resin bleed prevention effect, completes the present invention. That is, the present invention is as follows. 6 320190 200914568 (1) A resin bleed prevention agent comprising a ruthenium phosphate represented by the following formula: P(〇-(R2-0)n-R1)m ( 〇H) 3 m (wherein R! is a saturated or unsaturated hydrocarbon group having 4 to 30 carbon atoms, R2 is a lower stretching base, η is an integer of 0 to 1 ,, and 1 is an integer of 1 to 3). (2) The resin oozing prevention agent according to (1) above, wherein The oxime of the phosphate is any one of an alkyl group, an alkenyl group and an alkynyl group having a carbon number of 8 to 20, and R2 is an integer of from 1 to 6, and an integer of from j to 3. _ (3) The tree wax exudation preventing agent according to the above (1) or (2), further comprising: a nitrogen-containing heterocyclic compound containing any one of a tetra-salt derivative, a tri-salt derivative, a taste-suppressed derivative, and a samarium-salt derivative The discoloration preventing agent is a method of preventing the exudation of the resin by using the resin exudation preventing agent according to any one of the above (1) to (3). The substrate of the above-mentioned (1) to (7) is a film which prevents the treatment, and has a film for preventing the agent. (Effect of the Invention) The resin oozing prevention agent of the present invention is printed on the surface of the lead frame, and the surface of the body wiring substrate is adsorbed, and the resin oozing prevention effect or the smear prevention treatment of the smear is performed. Can not be damaged and discolored. In addition, the effect of the treatment is prevented to prevent the influence of the infiltration of the tree in the crystallizing step. Group characteristics such as wire bonding or mold sealing result in a small processing load. It is a non-gas-based resin bleed prevention agent, so drainage 320190 7 200914568 * [Embodiment] The resin bleed prevention agent of the present invention contains a phosphate represented by the following formula: 〇=P(〇-(R2-0)n -R1)m(〇H)3.m (wherein R! is a saturated or unsaturated hydrocarbon group having 4 to 30 carbon atoms, R2 is a lower alkyl group, η is an integer of 〇 to 1〇, and melon is 1 An integer to 3).

Ri為碳數4至30的飽和或不飽和之烴基。其中尤以 石炭數8至2G的飽和或不飽和之烴基為佳。若碳數過少則樹 脂滲出防止效果低，若過多則使模封性（模封樹脂之密 降低。 .. 就飽和或不飽和之烴基而言，可具有2個以上的雙 鍵、三鍵，此外，即使為直鏈狀亦可具有側鏈。再者，ς 狀烴基或芳族烴基亦可連結至主鏈，惟以直鏈 二 烯基、炔基為佳，以直鍵狀之燒基為尤佳。在稀基=基 中，雙鍵、三鍵的位置並無特別限制。 土 I為碳數1至4之低級伸烷基，以亞甲基 (methylene) Mt (ethylene) ^ ^ # , # ^ ^ n為0至10的整數 π f致马佳 m為1至3的整數。上述鱗酸酯中，單酿、二醋、 $曰2者皆為有用’獲得為混合物時不需要分離，可 混西物之形式來使用。此外，m為複數時，r、尺、; η可為不同。 12 本發明之㈣滲出防H容解於水等溶劑而作為相 320190 8 200914568 ^脂滲出防止劑溶液使用。上述樹脂渗出防止劑溶液中之上 ，述磷酸醋濃度以lmg/L至100g/L為佳，以i〇mg/L至離 為更佳。由於在上述濃度未達lmg/LBfRB〇防止效果弱， ^即使超過lOOg/L效果亦飽和而無法期待更高 為不佳。 再者，本發明之樹脂滲出防止劑可含有金屬之氧化變 止劑。就該變色防止劑而言，具體而言可使用公知之 〜防止劑’尤其是以含有四唾衍生物、三唾衍生物 :仃生物塞唑何生物之任一者的含氮雜環狀化合物變 色防止劑為佳。 夂 +就此等變色防止劑而言，可舉出例如四唾、苯并三哇、 本开咪唑、苯并噻唑、毓基苯并噻唑等。 上述變色防止劑係以在樹轉出防止劑溶液中含有1 L ^ 10〇g^# , , 1〇mg/L ^ 1〇g/L ^ 〇 ^ jlmg/L時變色防止效果弱’而即使超過⑽g/L效果 亦飽亡而無法期待更高的效果，故為不佳。 藉由含有變色防止劑，可予 屮 與變色防止效果。 仏#出防正效果 两，用水作為溶劑時，在上述碟酸醋不易溶於水時，可 添加醇、g同等有機溶劑。添加量雖可為上述鱗酸 須濃度’惟通常以〇ig/L至MOW為佳’ g —為更佳。若添加量過少則溶解性低，此外， 即使添加過多時溶解上述磷酸醋之效故卜 再者，在上述鱗酸醋不易溶於水時，可因應需要 it 320190 9 200914568 陰離子系、陽離子系、非離子系之界面活性劑之任一者； 或此等界面活性劑之混合物。其添加量可為丨至 l〇g/L ’宜為lOpg/L至ig/L。若添加量過少則溶解性低， 此外，即使添加過多時溶解上述鱗酸醋之效果亦不變，故 為不佳。 此外，在樹脂滲出防止劑溶液中，欲提升溶液 , -wv ^ η ^ ^ ρ±ι 緩衝性時，可因應需要添加01g/L至2〇〇岁1(宜為添加丄 至50g/L)之磷酸系、硼酸系、有機酸系之pH缓衝劑。若 未達〇.lg/L則PH緩衝效果低，即使超過2〇〇g/L效果亦飽 和而無法期待更高的效果，故為不佳。 此外，在樹脂滲出防止劑溶液中有金屬溶出時，可因 應需要而使用金屬遮蔽劑。就該金屬遮蔽劑而言，基本上 可使用公知者，尤其以使用胺系、胺錄酸系、羧酸系之 錯合劑為佳’添加量可為〇.lg/L jL2〇〇g/L，宜為_至 ，/L。若未達〇·! g/L貝金屬之錯合力低，即使超過·μ 效果亦飽和而無法期待更高的效果，故為不佳。 樹脂渗出防止劑溶液之ρΗ不需要特別限定，通常在 Τ至14。間，以在邱2至12處理為佳。若不在此範圍， 則素材的損傷大，樹脂滲出防止效果低。 行之轉出防止船讀之溫度以能財溶液進 广度乾圍，通常為5至9〇t，宜為1〇至_中 度過低則樹脂滲出防止效果彳 ’皿 合使作拿W ^ 此卜，即使超過9代也只 θ使作業性變差，提高温度並無助益。 再者，在樹脂滲出防止劑溶液之處理時間只要視效果 320190 10 200914568 在0·1秒至300秒適當調整即可，若考慮到作業之再現性 與效率㈣1秒至60秒為佳。若未達（Μ秒，則樹脂滲出 防止效果低，且作業之再現性變難，即使超過3⑼秒效果 亦飽和，且作業效率變低。 此外，本發明之樹脂滲出防止方法，係將配線基材浸 潰於樹月旨滲出防止劑溶液，或藉由淋浴、喷灑等方式將樹 月曰參出防止劑洛液散佈於基材，或藉由旋塗機等進行塗佈 使其接觸後，進行水洙、乾燥即可。 就配線基材而言’可舉出引線框架或印刷配線板等半 導體配線基材，以冰；隹^^、& 在進仃树知滲出防止處理之基材表面施 有金二銀、鈀、銅、鎳等鍍層者為佳。 猎由進行上述之樹脂彡出防止處理，而 =配線基材表面之電錢面，並形成由1至數分子左： 2 磷酸醋所構成的覆膜。因此，可使電鍍面盘黏晶 樹脂之接觸角增加，以 /、黏日日 ^ ^ ^ 忡制黏日日树月日之滲出。另外，由於 F特性不合酉曰覆膜非常薄’故對打線接合性、造膜性等組 、特丨生不會造成不好芬邀Ri is a saturated or unsaturated hydrocarbon group having 4 to 30 carbon atoms. Among them, a saturated or unsaturated hydrocarbon group having a charcoal number of 8 to 2 G is preferable. When the carbon number is too small, the resin bleed prevention effect is low, and if it is too large, the moldability (the density of the mold resin is lowered). The saturated or unsaturated hydrocarbon group may have two or more double bonds and three bonds. Further, it may have a side chain even in a linear form. Further, an anthracene hydrocarbon group or an aromatic hydrocarbon group may be bonded to the main chain, and a linear dienyl group or an alkynyl group is preferred, and a direct bond-like group is used. In the case of a dilute base, the positions of the double bond and the triple bond are not particularly limited. The soil I is a lower alkyl group having a carbon number of 1 to 4, and is a methylene Mt (ethylene) ^ ^ # , # ^ ^ n is an integer π f of 0 to 10, and Ma Jia m is an integer from 1 to 3. Among the above scales, single-brewed, di-vinegar, and $曰2 are all useful. It needs to be separated and can be used in the form of mixed western materials. In addition, when m is a complex number, r, the ruler, and η may be different. 12 (4) The osmotic anti-H solution is dissolved in a solvent such as water as a phase 320190 8 200914568 ^ The lipid exudation preventing agent solution is used. Above the resin exudation preventing agent solution, the concentration of the phosphoric acid vinegar is preferably from 1 mg/L to 100 g/L, and is from i〇mg/L to More preferably, since the above-mentioned concentration is less than 1 mg/LBfRB, the prevention effect is weak, and even if the effect exceeds 100 g/L, the effect is saturated and it cannot be expected to be higher. Further, the resin exudation preventing agent of the present invention may contain metal oxidation. In the case of the discoloration preventing agent, specifically, a known anti-inhibitor can be used, especially a nitrogen-containing one containing a tetrasalt derivative, a tris-salt derivative, or a biotinazole. The heterocyclic compound discoloration preventing agent is preferable. Examples of such discoloration preventing agents include tetrasodium, benzotrizene, benzimidazole, benzothiazole, mercaptobenzothiazole, and the like. The dosage system contains 1 L ^ 10〇g^# , 1〇mg/L ^ 1〇g/L ^ 〇^ jlmg/L in the tree-out prevention agent solution, and the discoloration prevention effect is weak' even if it exceeds (10) g/ The L effect is also too good to expect a higher effect, so it is not good. By containing a discoloration preventing agent, it is possible to prevent discoloration and discoloration. 仏#The anti-positive effect is two, and when water is used as a solvent, the above-mentioned disc acid When vinegar is not easily soluble in water, an alcohol or g equivalent organic solvent may be added. The above-mentioned scaly whisker concentration 'is usually 〇 ig / L to MOW is better ' g - is better. If the amount is too small, the solubility is low, and in addition, even if the addition is too much, the effect of dissolving the above-mentioned phosphoric acid vinegar is further When the above scaly vinegar is not easily soluble in water, any one of anionic, cationic or nonionic surfactants may be required according to it 320190 9 200914568; or a mixture of such surfactants. It can be from lOgg/L to lOpg/L to ig/L. If the amount is too small, the solubility is low, and the effect of dissolving the above scaly vinegar is not good even if it is added too much, so it is not good. . In addition, in the resin oozing inhibitor solution, when the solution is to be lifted, -wv ^ η ^ ^ ρ ± ι buffering, it is possible to add 01g/L to 2〇〇1 1 (preferably add 丄 to 50g/L) as needed. Phosphoric acid, boric acid, organic acid pH buffer. If it is less than lg.lg/L, the pH buffering effect is low, and even if the effect exceeds 2 〇〇g/L, the effect is saturated and a higher effect cannot be expected, which is not preferable. Further, when metal is eluted in the resin bleeding prevention agent solution, a metal shielding agent can be used as needed. As the metal masking agent, it is basically possible to use a known one, and it is preferable to use an amine-based, aminic acid-based or carboxylic acid-based complexing agent. The amount of addition can be 〇.lg/L jL2〇〇g/L. , should be _ to, /L. If it is not reached, the g/L shell metal has a low combined force, and even if the effect exceeds the μ, the effect is saturated and a higher effect cannot be expected, so it is not good. The ρ Η of the resin bleed prevention agent solution is not particularly limited and is usually Τ to 14. It is better to deal with it in Qiu 2 to 12. If it is not in this range, the damage of the material is large, and the resin bleed prevention effect is low. The transfer of the line prevents the temperature of the ship from entering the breadth of the energy solution, usually 5 to 9 〇t, preferably 1 〇 to _ moderately low, the resin oozing prevention effect 彳 '皿合作作作W ^ Therefore, even if it exceeds 9 generations, only θ deteriorates workability, and it is not helpful to increase the temperature. Further, the treatment time of the resin bleed prevention agent solution may be appropriately adjusted as long as the effect 320190 10 200914568 is from 0.1 second to 300 seconds, and it is preferable to consider the reproducibility and efficiency of the work (4) from 1 second to 60 seconds. If it is not reached (the second generation, the resin bleed prevention effect is low, and the reproducibility of the work becomes difficult, and the effect is saturated even if it exceeds 3 (9) seconds, and the work efficiency is lowered. Further, the resin bleed prevention method of the present invention is a wiring base. The material is immersed in the sap exudation preventing agent solution, or the saplings of the saplings are sprayed on the substrate by showering, spraying, or the like, or coated by a spin coater or the like. In the case of the wiring substrate, a semiconductor wiring substrate such as a lead frame or a printed wiring board can be cited as ice; 隹^^, & The surface of the material is preferably coated with gold, silver, palladium, copper, nickel, etc. Hunting is carried out by performing the above-mentioned resin removal prevention treatment, and = the surface of the wiring substrate is formed by 1 to several molecules left: 2 A film made of phosphoric acid vinegar. Therefore, the contact angle of the die-cast resin of the plated face plate can be increased, and the viscous day and day of the tree can be oozing out.酉曰The film is very thin, so it is suitable for wire bonding and film forming. Group, special Shu-fen invite students will not cause bad

效果或封孔處理效果。以：二L 而# ^斗 文果以上述方法施行樹脂滲出防止處理 = = 覆膜的配線基材、以及使用該配隸 封裝亦包含在本發明中。 黏晶發明之樹脂渗出防止處理後所使用的 脂，可舉出W脂而言，可為低應力型之黏晶樹 佳。 衣乳樹脂、丙烯酸系樹脂等，且以環氧樹脂為 320190 11 200914568 '(實施例） 以下’雖根據貫施例說明本發明，惟本發明非限定於 此等實施例者。 、 實施例1至6，比較例1至2 為了在銅合金（Cu : 97.7%、Sn : 2.0%、Ni : 0.2%、p : 0.03%)製引線框架提升密著性而進行銅打底電鍍&⑴^ plating)作為底層後，於引線框架全面施以鍍銀、鍍金、鍍 銅之任一者。藉由浸潰而進行記載於之後表丨的樹脂滲出 防止處理。 / 針對此等基材，進行黏晶，並進行耐樹脂滲出性（你 RBO性）、打線接合性（W/B性）、模封性、耐變色性之評估| 將結果顯示於表卜表1中，電鍍浴組成中之「__」°表# 不添加，在評估攔之「―」表示在評估對象之外。」π L表1中之Rl、R2、η係表示上述通式所示之璃 -酉曰中的Rn η ’磷酸酯係使用單酯與二酯之！ it:;使磷酸醋之Rl的燒基、缔基全部為直鏈狀， •^例5、6中_基為在中央具有雙鍵之 11-二十二烯基。 卞埤暴、 耐樹脂滲出性之評估係以下述方法進行。 將市面販售之低應力黏晶用環氧樹月旨 (ABLEBOND834()，織她社製）塗佈於經進 防止處理的電鍍面後，在大氣中，以室 月曰：ti 著，在大氣令以熱板進行、'】 小日'。^ 屬顯微鏡（100件）#Θ t ^ T的熱硬化後，以: )親純氧樹腊塗佈部，如第 320190 12 200914568 樹脂滲出最嚴重部分的滲出量（RB 0量），以如下方式進行 評估。 〇：未達ΙΟμπι △ : ΙΟμιη以上，且未達50μπι X : 50μιη 以上 打線接合性之評估係以下述方法進行。 使用25μπι金線，以超音波併用熱壓著方式（溫度：200 °C、荷重：50g、時間：10ms)進行打線接合，並以拉力測 試機（pull tester)測試拉力強度，以如下方式進行評估。 〇：10gf以上 X :未達10gf 模封性之評估係以下述方法進行。 將市面販售之模封用環氧樹脂（住友BAKELITE製， EME-6300)塗佈於經進行樹脂滲出防止處理的電鍍面後， 進行175°C、5小時的熱硬化，之後測定密著性（剪切強度）， 以如下方式進行評估。 〇：20kgf/cm2 以上 △ : 10 kgf/cm2 以上，且未達 20 kgf/cm2 X :未達 10 kgf/cm2 耐變色性之評估係以下述方法進行。 以40°C、溼度90%加溼96小時後，進行外觀觀察， 並如以下方式進行評估。 〇：無變色 X :有變色 13 320190 200914568 [表 1-1] 實施例 1 2 3 4 基材或電銀表面 銀 銀 銀 銀 主成分R1 c6h13 c8h17 Cl2H25 Cl6H33 R2 — . — ch2ch2 ch2ch2 η 0 0 2 2 濃度 0.5g/L 0.5g/L 0.5g/L 0.5g/L 變色防止劑 — — — 酼基苯并噻 唑：0.1g/L 電鍍浴組成 溶劑 — — — 異丙醇：5g/L pH緩衝劑 四棚酸鉀： Ir/L — 焦磷酸鉀： lg/L — 錯合劑 — 伸乙二胺四乙 酸四鈉：lg/L — — 界面活性劑 — 氧伸乙基壬基 苯基趟：lmg/L — — pH 9.0 9.0 9.0 9.0 處理條件 處理溫度 (°C) 25 25 25 25 處理時間 ⑻ 10 10 10 10 RBO性 Δ 〇 〇 〇 5平估結果 W/B性 〇 〇 〇 〇 模封性 〇 〇 〇 〇 财變色性 〇. 〇 〇 〇 14 320190 200914568 [表 1-2] 實施例 比較例 5' 6 1 2 基材或電鍍表面 金 銅 銀 銀 電鍍浴 組成 主成分R1 C20H39 C22H43 c3H7 C32H65 R2 ch2ch2 ch2ch2 -— ch2ch2 η 3 4 0 8 濃度 0.5g/L 0.5g/L 0.5g/L 0.5g/L 變色 防止劑 一 苯并三唾： 0.1 g/L — — 溶劑 異丙醇： l〇g/L 異丙醇：10g/L — 異丙醇： l〇g/L pH緩衝劑 罐酸卸：lg/L — — — 錯合劑 — 伸乙二胺四乙 酸四鈉：lg/L — — 界面 活性劑 — — — — 處理條件 pH 9.0 9.0 9.0 9.0 處理溫度 CC) 25 25 25 25 處理時間 ⑻ 10 10 10 10 5平估結果 RBO性 〇 〇 X 〇 W/B性 〇 — 〇 X 模封性 〇 Δ 〇 X 耐變色性 〇 〇 〇 〇 【圖式簡單說明】 第1圖係表示實施例之耐樹脂滲出性評估中之樹脂滲 出量之測定方法的圖。 【主要元件符號說明】 無 15 320190Effect or sealing effect. In the present invention, the resin substrate is subjected to the resin bleeding prevention treatment by the above method. = = The wiring substrate of the film and the use of the package are also included in the present invention. The grease used in the resin osmosis prevention treatment of the viscous crystal invention is preferably a low-stress type viscous crystal. Latex resin, acrylic resin, etc., and epoxy resin 320190 11 200914568 '(Examples) Hereinafter, the present invention will be described based on the examples, but the present invention is not limited to the examples. Examples 1 to 6, Comparative Examples 1 to 2 In order to improve the adhesion of the lead frame in a copper alloy (Cu: 97.7%, Sn: 2.0%, Ni: 0.2%, p: 0.03%), copper plating was performed. & (1)^ plating) After the bottom layer, the lead frame is entirely coated with silver, gold plating, or copper plating. The resin bleeding prevention treatment described in the subsequent surface is performed by dipping. / For these substrates, perform die-bonding, and perform evaluation of resin-resistant exudation (your RBO property), wire bonding (W/B property), moldability, and discoloration resistance. The results are shown in the table. In 1st, the "__" in the composition of the plating bath is not added, and the "-" in the evaluation block indicates that it is outside the evaluation object. In the case of π L, R1, R2 and η represent the Rn η ' phosphate ester of the glass of the above formula, using a monoester and a diester! It:; the base of the R1 of the phosphoric acid vinegar and the base group are all linear, and the group of the examples 5 and 6 is an 11-dodecadienyl group having a double bond at the center. The evaluation of hailstorm and resin bleed resistance was carried out in the following manner. The low-stressed viscous crystals that are sold in the market are coated on the plating surface of the anti-inhibition treatment by the epoxy resin ( ABLEBOND 834 (), manufactured by Kosei Co., Ltd.), and then in the atmosphere, in the atmosphere, ti: The atmosphere is made by hot plates, '] small day'. ^ Microscope (100 pieces) #Θ t ^ T After thermal hardening, to: ) Pro-oxygen wax coating section, such as 320190 12 200914568 resin exudation of the most severe part of the amount of exudation (RB 0 amount), as follows Ways to evaluate. 〇: Not up to πμπι Δ : ΙΟμιη or more, and less than 50 μπι X : 50 μιη or more The evaluation of the wire bonding property was carried out by the following method. Using 25 μπι gold wire, ultrasonic bonding and hot pressing (temperature: 200 ° C, load: 50 g, time: 10 ms) were used for wire bonding, and the tensile strength was measured by a pull tester, and evaluated as follows. . 〇: 10 gf or more X: Evaluation of less than 10 gf of moldability was carried out in the following manner. The epoxy resin for mold sealing (manufactured by Sumitomo BAKELITE, EME-6300) was applied to a plating surface subjected to resin bleeding prevention treatment, and then heat-hardened at 175 ° C for 5 hours, and then the adhesion was measured. (Shear strength), evaluated in the following manner. 〇: 20 kgf/cm2 or more △ : 10 kgf/cm2 or more, and less than 20 kgf/cm2 X: less than 10 kgf/cm2 The evaluation of the discoloration resistance was carried out by the following method. After humidification at 40 ° C and a humidity of 90% for 96 hours, the appearance was observed and evaluated as follows. 〇: no discoloration X: discoloration 13 320190 200914568 [Table 1-1] Example 1 2 3 4 Substrate or electro-silver surface silver silver silver main component R1 c6h13 c8h17 Cl2H25 Cl6H33 R2 — . — ch2ch2 ch2ch2 η 0 0 2 2 Concentration 0.5g/L 0.5g/L 0.5g/L 0.5g/L Discoloration inhibitor — — — Mercaptobenzothiazole: 0.1g/L Electroplating bath Composition solvent — — — Isopropanol: 5g/L pH buffer Potassium tetra-sulphate: Ir/L - potassium pyrophosphate: lg/L - mis-agent - tetrasodium ethylenediaminetetraacetate: lg / L - surfactant - oxygen extended ethyl mercapto phenyl hydrazine: lmg /L — — pH 9.0 9.0 9.0 9.0 Processing conditions Processing temperature (°C) 25 25 25 25 Processing time (8) 10 10 10 10 RBO Δ 〇〇〇5 flattening result W/B 〇〇〇〇 〇〇〇〇 〇 〇变色14 320190 200914568 [Table 1-2] Example Comparative Example 5' 6 1 2 Substrate or plated surface Gold-copper silver-silver plating bath Composition principal component R1 C20H39 C22H43 c3H7 C32H65 R2 ch2ch2 ch2ch2 -— ch2ch2 η 3 4 0 8 Concentration 0.5g/L 0.5g/L 0.5g/L 0.5g/L Discoloration Preventive agent monobenzotriazine: 0.1 g/L — solvent isopropanol: l〇g/L isopropanol: 10g/L — isopropanol: l〇g/L pH buffer tank acid unloading: lg/ L — — — Wrong agent — tetrasodium ethylenediaminetetraacetate: lg/L — — surfactant — — — — Processing conditions pH 9.0 9.0 9.0 9.0 Processing temperature CC) 25 25 25 25 Processing time (8) 10 10 10 10 5 flattening result RBO 〇〇X 〇W/B 〇 〇 〇X Molding 〇Δ 〇X Resistance to discoloration 〇〇〇〇 [Simple description of the drawing] Fig. 1 shows the resin bleed resistance of the example A diagram for the measurement method of the amount of resin exudation in the evaluation. [Main component symbol description] None 15 320190

Claims (1)

200914568 十、申請專利範圍： ' L 一種樹脂滲出防止劑’包含以下述通式表示之磷酸酯 〇=P(0-(R2-0)n-R1)m(OH)3.m (式中尺1為兔數4至30的飽和或不飽和之煙基，r, 為低級伸烷基’n為〇至10的整數，m為〗至3的整數 2.如申明專利範圍第1項之樹脂滲出防止劑，其中，上述 磷酸酯之Rl為碳數δ S 20的烧基、縣、块基之任丄 者尺2為伸乙基，整數，瓜為^至 數。 J ^ ^請專㈣㈣〗項或f 2項之樹轉 包含··含有四唾衍生物、三唾衍生物、味 ^ 唑衍生物之任一者的含氮啤产人 生物、噻 4· 一種樹脂滲出防止方法，孫 色防止劑。 料扭s 使用申請專利範圍第1至3 財任-項之樹轉出^劑施以樹躲 至3 種基材，係經使用申請專利範圍第^ 處理。 之樹脂滲出防止劑施以樹脂滲出射任-項 脂滲出防止劑之覆膜。 恿理，而具有該樹 320190 16 200914568 七、 指定代表圖： (一） 本案指定代表圖為：第（1 )圖。 (二) 本代表圖之元件符號簡單說明： 無元件符號 八、 本案若有化學式時，請揭示最能顯示發明特徵的化學式： 本案無代表化學式 4 320190200914568 X. Patent application scope: 'L A resin bleed out preventer' contains a phosphate 〇=P(0-(R2-0)n-R1)m(OH)3.m expressed by the following formula (in the formula) 1 is a saturated or unsaturated smoky group of 4 to 30 rabbits, r, is a lower alkylene group 'n is an integer from 〇 to 10, and m is an integer from 〖 to 3. 2. Resin according to claim 1 of the patent scope The exudation preventing agent, wherein R1 of the above phosphate ester is a burning group of a carbon number of δ S 20 , and a ruler of a county or a block base is a stretched ethyl group, an integer, and a melon is a number to a number. J ^ ^ Please (4) (4) The item or the f2 item tree includes: a nitrogen-containing beer producing organism containing any of a tetra-salt derivative, a tri-salt derivative, and a sulphur-like azole derivative, and a thiophene 4 Color preventive agent. Material twisted s Use the patent scope of the first to third fiscal-item tree transfer agent to apply the tree to the three kinds of substrates, which are used in the patent application scope. Applying a resin to bleed out the film of the anti-lipid exudation preventing agent. 恿理,有有树320190 16 200914568 VII. Designated representative figure: (1) The case The designated representative figure is: (1). (2) The symbol of the symbol of the representative figure is simple: No component symbol 8. If there is a chemical formula in this case, please disclose the chemical formula that best shows the characteristics of the invention: This case does not represent the chemical formula 4 320190
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