TW200907107A - Surface treating agent - Google Patents
Surface treating agent Download PDFInfo
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- TW200907107A TW200907107A TW097124748A TW97124748A TW200907107A TW 200907107 A TW200907107 A TW 200907107A TW 097124748 A TW097124748 A TW 097124748A TW 97124748 A TW97124748 A TW 97124748A TW 200907107 A TW200907107 A TW 200907107A
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- surface treatment
- treatment agent
- acid
- compound
- zinc
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/22—Secondary treatment of printed circuits
- H05K3/28—Applying non-metallic protective coatings
- H05K3/282—Applying non-metallic protective coatings for inhibiting the corrosion of the circuit, e.g. for preserving the solderability
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- 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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/52—Treatment of copper or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D235/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings
- C07D235/02—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings condensed with carbocyclic rings or ring systems
- C07D235/04—Benzimidazoles; Hydrogenated benzimidazoles
- C07D235/06—Benzimidazoles; Hydrogenated benzimidazoles with only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, directly attached in position 2
- C07D235/08—Radicals containing only hydrogen and carbon atoms
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/22—Secondary treatment of printed circuits
- H05K3/28—Applying non-metallic protective coatings
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
- B23K35/262—Sn as the principal constituent
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
- H05K2203/12—Using specific substances
- H05K2203/122—Organic non-polymeric compounds, e.g. oil, wax, thiol
- H05K2203/124—Heterocyclic organic compounds, e.g. azole, furan
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
Description
200907107 九、發明說明： ，【發明所屬之技術領域】 本發明是有關於一種表面處理劑。更詳細而言，關於 一種用於處理基材表面的表面處理劑，上述基材具有包含 銅或銅合金的表面。 【先前技術】 一直以來，作為用於包含銅或銅合金的配線電路的防 銹或提高共熔焊錫性的表面處理劑，日本專利特開平 5-163585號公報、日本專利特開平5_237688號公報、曰本 專利特開平7-54169號公報以及日本專利特開平 1M77218號公報中公開了包含苯並咪唑等咪唑化合物的 水溶性預焊劑(Organic Solderability Preservative, OSP)。 但 近年來’從環境角度考慮大多使用無鉛焊錫。無錯焊 錫與以往的共晶焊錫相比熔點高，因此必需在高溫下進行 共熔焊錫(eutectic solder)。因此，使用無鉛焊錫進行共熔 焊錫時要求所用表面處理劑所形成的覆膜具耐熱性。^為 形成耐熱性優異的覆膜的表面處理劑，曰本專利特開& =584號公報中公開了含有鋅化合物的表面處理劑^ 1發由明上内述1面處理劑形成的覆膜的耐熱性還不能說充分 不禮料上述财技摘設，其目料於提供一種 =用現有的共晶焊錫進行聽焊錫時可以使用、使用 …鉛焊錫進行共熔焊錫時也可以使用、 覆膜的表面處理劑。 $成耐熱性優異的 200907107 根據本發明’提供一種表面處理劑，其用於處理包含 銅或銅合金之基材之表面，絲面處理射含有_嗤化合 物及糖醇的溶液，上述溶液中含有鋅離子。 >為讓本發明之上述和其他目的、特徵和伽能更明顯 易懂’下文特舉較佳實麵，並配合觸㈣，作詳細 明如下。 【實施方式】 本發明之表面處理劑包含咪唑化合物以及糖醇的溶 液，並含有鋅離子。 、、咪唑化合物的例子有：2_丙基苯並咪唑、2_環己基苯 並味，、2·苯基苯並咪哇、2•节基笨並#唾、2_(3·苯丙基 甲基苯並咪唑、2-(巯基曱基)苯並咪唑、2_(1-萘甲基)苯並 〇米°坐、2<5，'苯基)戊基苯並p米唑、2-苯乙基苯並味唑、5-，2 丁基本並味唾等苯並味唾化合物；二苯基-甲基 米坐2-戊基味哇、2·_{燒基-4-甲基咪峻、2,4-二甲基味 ，、2,4-二苯基咪唑、2,4,5_三苯基咪唑、2•苄基咪唑、厶 苄基-4·甲基咪唑等其他咪唑化合物等。上述咪唑化合物各 自可以單獨使用，也可以是兩種或兩種以上併用。 同覆膜形成性的觀點考慮，本發明之表面處理劑 中咪唑化合物的濃度較佳的是大於等於0.01重量百分比 、wtj) ’更佳的是大於等於〇 〇5减％。從使咪唾化合物充 分溶解於本發明之表面處理财，提高本㈣之表面處理 d之均勻性的觀點考慮"㈣化合物的濃度較佳的是小於 等於5 wt%’更佳的是小於等於丨wt%。從上述觀點考慮， 200907107 ====合物的濃度較佳的是。 溶出的銅離子結合，因此本發明面處理剩中 銅合金的基材上的覆膜形成性得以提高包含銅或 異種金屬上形成覆膜。 q同㈠'可以抑制於 用於處理劑用於製造印刷配線板時，可以 = 合金的配線電路的防銹或提高共炫2 f印刷配線板上的包含銅的配線中，有時會 銀、#、錫等除銅以外的金 二金、 的包括口米峻化合物的表面處二，種情況下’使用叫 覆媒’因此表面處理劑的覆種金屬表面也形成 當使用本《之心m時相對於此， 的變色。 叶了以抑制表面處理劑之覆膜200907107 IX. Description of the invention: [Technical field to which the invention pertains] The present invention relates to a surface treatment agent. More specifically, with respect to a surface treatment agent for treating the surface of a substrate, the above substrate has a surface containing copper or a copper alloy. [Prior Art] As a surface treatment agent for rust-preventing or eutectic soldering of a wiring circuit including copper or a copper alloy, Japanese Patent Laid-Open No. Hei 5-165835, Japanese Patent Laid-Open No. Hei No. Hei-5-237688, An organic Solderability Preservative (OSP) containing an imidazole compound such as benzimidazole is disclosed in Japanese Laid-Open Patent Publication No. Hei. No. Hei. No. Hei. However, in recent years, most lead-free solders have been used from an environmental point of view. Improper soldering has a higher melting point than conventional eutectic solders, so it is necessary to perform eutectic solder at high temperatures. Therefore, when a eutectic solder is used for eutectic soldering, it is required that the film formed by the surface treating agent used has heat resistance. In order to form a surface treatment agent for a film having excellent heat resistance, a surface treatment agent containing a zinc compound is disclosed in Japanese Laid-Open Patent Publication No. 584, and a coating formed by the one-side treatment agent described above is disclosed. The heat resistance of the film cannot be said to be sufficiently inconspicuous. The purpose of the film is to provide a kind of = can be used when using existing eutectic solder for soldering, and can be used when using eutectic solder for lead solder. A surface treatment agent for the film. 200907107 which is excellent in heat resistance according to the present invention' provides a surface treatment agent for treating a surface of a substrate comprising copper or a copper alloy, and the surface treatment comprises a solution containing a cerium compound and a sugar alcohol, and the solution contains Zinc ions. The above and other objects, features and gamma of the present invention are more apparent and understood. The following detailed description will be given in detail, and in conjunction with the touch (four), the details are as follows. [Embodiment] The surface treatment agent of the present invention contains a solution of an imidazole compound and a sugar alcohol, and contains zinc ions. Examples of the imidazole compound are: 2-propylbenzimidazole, 2-cyclohexylbenzaldehyde, 2·phenylbenzimid, 2·node stupid and #sal, 2_(3·phenylpropyl) Methylbenzimidazole, 2-(indolyl)benzimidazole, 2-(1-naphthylmethyl)benzopyrene, 2<5, 'phenyl)pentylbenzopyrimazole, 2- Phenylethyl benzoxazole, 5-, 2-butyl benzoate and other benzo-salt compounds; diphenyl-methyl rice sit 2-pentyl-flavored, 2·_{alkyl-4-methyl Mi Jun, 2,4-dimethyl taste, 2,4-diphenylimidazole, 2,4,5-triphenylimidazole, 2•benzylimidazole, benzylbenzyl-4·methylimidazole, etc. Imidazole compounds and the like. These imidazole compounds may be used singly or in combination of two or more kinds. The concentration of the imidazole compound in the surface treatment agent of the present invention is preferably 0.01% by weight or more, wtj)', more preferably 大于55% or less, from the viewpoint of film formability. From the viewpoint of sufficiently dissolving the sodium saliva compound in the surface treatment of the present invention and improving the uniformity of the surface treatment d of the present invention (4), the concentration of the compound is preferably 5% or less by weight, and more preferably less than or equal to丨wt%. From the above viewpoints, the concentration of the 200907107 ==== compound is preferably. Since the eluted copper ions are bonded, the film formation property on the substrate on which the copper alloy is left to be treated in the present invention is improved to include a film formed on copper or a dissimilar metal. q (1) can be suppressed when the processing agent is used to manufacture a printed wiring board, and the wiring of the alloy can be rust-proof or the copper-containing wiring on the printed circuit board can be increased. #,锡等, etc. in addition to copper, the surface of the gold-containing gold, including the surface of the compound, is in the second case, the use of the coating medium, so the surface of the surface treatment agent is also formed when using the heart of the m In contrast to this, the discoloration. Leaf to inhibit the surface treatment agent
並且，在本發明之表面處理劑中，由於 ==力Τ子螯合劑作為抑制在上述異種金屬I 時=，理,具二=:成覆膜 糖醇的例子包括：甘靈龄 醇、麥芽糖醇、乳糖醇等單糖醇=醇、木糖醇、赤蘚糖 醇等多糖醇等。上述糖醇可糖等二糖醇；低聚糖 種或兩種以上併用。在上述早獨使用，也可以是兩 在上述糖醇中，從能夠抑制在金等異 200907107 種金屬上形顧_觀財慮，健 梨醇以及木糖醇所組成的組群中的至少一種。路·、山 從提高包含本發明之表面處理劑之 點考慮’本發明之表面處_+糖2、較佳二大， 更佳的是大於等於。，二= 的疋大於等於0.1 wt% ;從經濟性的 較佳的是小於等於7 wt%’更佳的是慮’糖^辰度 更住的疋小於等於4 wt%，進Further, in the surface treatment agent of the present invention, since the == force chelating agent is inhibited as the above-mentioned dissimilar metal I, the following examples include: ganol alcohol, maltitol, Monosaccharide alcohol such as lactitol = polysaccharide alcohol such as alcohol, xylitol or erythritol. The above-mentioned disaccharide alcohol such as sugar alcohol saccharide; oligosaccharide species or a combination of two or more. In the above-mentioned sugar alcohol, it is also possible to prevent at least one of the group consisting of sorbitol and xylitol in the above-mentioned sugar alcohol, which is capable of suppressing the formation of various metals such as gold. . From the viewpoint of improving the surface treatment agent of the present invention, the surface of the present invention is _+2, preferably 2, more preferably greater than or equal to. The 疋 of the two = is greater than or equal to 0.1 wt%; the economical preference is preferably less than or equal to 7 wt%, and it is better to consider that the sugar is more than or equal to 4 wt%.
-^紅的是小於等於丨wt%。從上顿點考慮，本發明 之衣面處理劑中糖醇濃度較佳的是〇 〇1〜7研％， 是0.05〜4树％，進一步較佳的是〇·1〜1 wt%。 ’ 咪唑化合物及糖醇的溶液可以藉由將咪唑化合物及糖 醇溶解於溶劑中來進行製備。 /谷劑的例子包括.離子交換水、純水、超純水等水； 有機酸、無機酸等酸；水溶性有機溶劑等。上述溶劑中， 從促進咪唑化合物溶解的觀點考慮’較佳的是酸以及水溶 性有機溶劑。-^ Red is less than or equal to 丨wt%. From the viewpoint of the above, the concentration of the sugar alcohol in the coating treatment agent of the present invention is preferably from 〜1 to 7% by mol, and is preferably from 0.05 to 4% by weight, more preferably from 1 to 1% by weight. The solution of the imidazole compound and the sugar alcohol can be prepared by dissolving the imidazole compound and the sugar alcohol in a solvent. Examples of the granules include water such as ion-exchanged water, pure water, and ultrapure water; acids such as organic acids and inorganic acids; and water-soluble organic solvents. Among the above solvents, from the viewpoint of promoting dissolution of the imidazole compound, an acid and a water-soluble organic solvent are preferred.
酸包括有機酸及無機酸。有機酸及無機酸各自可以單 獨使用，也可以併用。 有機酸的例子包括：曱酸、乙酸、丙酸、經基乙酸、 正丁酸、異丁酸、丙烯酸、巴豆酸、異巴豆酸、草酸、丙 一酸、墟拍酸、己一酸、馬來酸、乙块二幾酸、一氯乙酸、 二乳乙酸、一漠乙酸、乳酸、氧基丁酸、甘油酸、酒石酸、 蘋果酸、枸櫞酸、庚酸、己酸等。上述有機酸各自可以單 獨使用’也可以是兩種或兩種以上併用。 200907107 、、無機酸的例子包括：鹽酸、硫酸、硝酸、磷酸等。上 述無機酸各自可以單獨使用，也可以是兩種或兩種以上併 用。 需要說明的是，咪唑化合物相對於酸的溶解度因咪唑 化合物及酸的種類而異’故較佳的是，根據咪唑化合物的 種類來選擇酸的種類及其量。 從使味《坐化合物充分溶解的觀點考慮，本發明之表面 處理劑中酸的濃度較佳的是大於等於1 wt%，更佳的是大 於等於1.5 wt%，進一步較佳的是大於等於3 wt%。從提高 本發明之表面處理劑之覆膜彤成性的觀點考慮，本發明之 表面處理劑中酸的濃度較佳的是小於等於80 wt%，更佳的 是小於等於50 wt。/。，進一步較佳的是小於等於3〇树％。 從上述觀點考慮，本發明之表面處理劑中酸的濃度較佳的 是1〜80 wt% ’更佳的是1.5〜50加％，進一步較佳的是3 〜30 wt%。 水溶性有機溶劑的例子包括：甲醇、乙醇、異丙醇、 乙二醇單甲醚、乙二醇單乙_。從使料化合物充分溶 解的觀點考慮，本發明之表面處理射水雜有 濃度較佳的是大料於〗wt%，更佳岐切=7^ wt% ’進-辣佳岐切等於3 wt%。從提高本發明之 表面處理劑之覆臈形成性的觀點考慮，本發明之表理 劑中水溶性有機溶劑的濃度較佳的是小於等於80wt% 佳的是小於料3G Wt%，進—步難蚊小於15 wt%。從上述觀點考慮’本翻之表面處理劑巾的水溶性 200907107 有機溶劑的濃度較佳的是1〜80 wt%，更佳的是】5〜3 wt%，進一步較佳的是3〜15 wt°/〇。 〇 調整本發明之表面處理劑中的溶劑量，使本發明之表 面處理劑中含有所需濃度的咪唑化合物、糖醇及鋅離子广Acids include organic acids and inorganic acids. The organic acid and the inorganic acid may each be used singly or in combination. Examples of organic acids include: citric acid, acetic acid, propionic acid, transacetic acid, n-butyric acid, isobutyric acid, acrylic acid, crotonic acid, isocrotonic acid, oxalic acid, propionic acid, ruthenium acid, hexanoic acid, horse Toluene, a block of diacid, monochloroacetic acid, diacetic acid, a desert acetic acid, lactic acid, oxybutyric acid, glyceric acid, tartaric acid, malic acid, citric acid, heptanoic acid, caproic acid and the like. Each of the above organic acids may be used singly or in combination of two or more. 200907107, examples of inorganic acids include: hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, and the like. Each of the above inorganic acids may be used singly or in combination of two or more kinds. In addition, the solubility of the imidazole compound with respect to an acid differs depending on the kind of the imidazole compound and the acid. Therefore, it is preferred to select the type and amount of the acid depending on the type of the imidazole compound. The concentration of the acid in the surface treatment agent of the present invention is preferably 1 wt% or more, more preferably 1.5 wt% or more, and still more preferably 3 or more, from the viewpoint of sufficiently dissolving the taste compound. Wt%. The concentration of the acid in the surface treating agent of the present invention is preferably 80% by weight or less, more preferably 50% or less, from the viewpoint of improving the film formation property of the surface treating agent of the present invention. /. Further preferably, it is less than or equal to 3% of eucalyptus. From the above viewpoints, the concentration of the acid in the surface treating agent of the present invention is preferably from 1 to 80% by weight, more preferably from 1.5 to 50% by weight, still more preferably from 3 to 30% by weight. Examples of the water-soluble organic solvent include methanol, ethanol, isopropanol, ethylene glycol monomethyl ether, and ethylene glycol monoethyl _. From the viewpoint of sufficiently dissolving the compound, the surface treatment jet of the present invention preferably has a concentration of more than 〖wt%, more preferably 岐========================================== . The concentration of the water-soluble organic solvent in the surface agent of the present invention is preferably 80% by weight or less, preferably less than 3G Wt%, from the viewpoint of improving the coverage of the surface treating agent of the present invention. Difficult mosquitoes are less than 15 wt%. From the above viewpoints, the concentration of the water-soluble 200907107 organic solvent of the surface treatment agent of the present invention is preferably from 1 to 80% by weight, more preferably from 5 to 3% by weight, still more preferably from 3 to 15% by weight. °/〇. 〇 adjusting the amount of the solvent in the surface treating agent of the present invention so that the surface treating agent of the present invention contains a desired concentration of an imidazole compound, a sugar alcohol, and a zinc ion.
U 就鋅離子而言，例如藉由使用在溶解於本發明之表 處理劑所用之成分中時產生鋅離子的化合物，可以使本發 明之表面處糊巾含有鋅離子。「在溶解於該表面處理劑^ 用之成分巾魅生鋅離子的化合物」是指町「產生辞離 子的化合物」。產生鋅離子的化合物較佳的是容易被本發明 之表面處理劑中所用之成分溶解的鋅化合物。例如當^發 明之表面處理射包含醋酸時，由於醋_祕於醋酸， 因此其是較佳的產生鋅離子的化合物。 產生鋅離子的化合物的例子包括：氧化辞、醋酸辞、 甲酸鋅m硫畴 '雜鋅、·料。上述產生 =離子的化合物各自可以單獨使用，也可以是兩種或兩種 併用在產生鋅離子的化合物中，從溶解性良好、可 =;液中敎存在的角度考慮，較佳的是I氧了 酷酸鋅及甲酸鋅所組成的組群中的至少一種。 鋅離子可以藉由將魅㈣子的化合物溶解於上述溶 釗中而生成。 翻Et 2提同由本發明之表面處_形成的覆麟财熱性的 ^慮’本發明之表面處理射_子的濃度較佳的是 ^ 4於⑽3 Wt%，更佳的是大於等於0.1 wt%，進-步 較佳的是大於等於G.2 wt%。從提高咪舰合物的溶解性 10 200907107 的觀點考慮，鋅離子遭度較佳 上述觀點考慮，本發明之 ★疋小於等於0.5 wt%。從 的是〜〇.5㈣，更料^理财_子的漠度較佳 的是0.2〜0.5研％。 疋.3〜0.5 ，進一步較佳 需要說明的是，本發明 意思是指求出本發明之表劑的鋅離子濃度 的溶解量中的鋅量，由上 生，子的化合物 而求得的值。 —除以衣面處理劑總體的量 及產合物、糖醇 行製備。將蜂哇化合物、糖醇及來容易地進 溶劍，沒有特別限定於溶劑時的 而要巩明的是，為了提高本 鋼或銅合金的基材表面的覆膜形成性，在本=劑在包含 理劑中可以含有銅離子。 本卷月之表面處 有覆二=3:::加:據需要更可以含 銅或如有以 二包括,硬 、面处理射適用於印刷配線板之銅電路部。銅各金 是包括大於等於50 wt%的銅和小於等於5〇祕的 錫、金、銀、鋁等除銅以外的金屬。 將本發明之表面處理劑應用於基材時，表面處理劑的U In the case of zinc ions, for example, by using a compound which generates zinc ions when dissolved in a component used in the treatment agent of the present invention, the surface of the paste of the present invention may contain zinc ions. "A compound which dissolves in the surface treatment agent and which is used to smear zinc ions" means "a compound which produces a dissociation". The zinc ion-generating compound is preferably a zinc compound which is easily dissolved by the components used in the surface treating agent of the present invention. For example, when the surface treatment of the invention comprises acetic acid, it is a preferred compound for generating zinc ions since vinegar is secreted from acetic acid. Examples of the compound which generates zinc ions include: oxidized words, acetic acid, zinc formate m-sulfur domains, 'di-zinc, and materials. The above-mentioned compounds which generate ions may be used singly or in combination of two or two kinds of compounds for generating zinc ions. From the viewpoint of good solubility, and the presence of ruthenium in the liquid, I oxygen is preferred. At least one of the group consisting of zinc silicate and zinc formate. Zinc ions can be formed by dissolving a compound of the genus (tetra) in the above solution. The concentration of the surface treatment emitter of the present invention is preferably (4) 3 Wt%, more preferably 0.1 wt% or more, which is formed by the surface of the present invention. %, the step-by-step is preferably greater than or equal to G.2 wt%. From the viewpoint of improving the solubility of the imidate compound 10 200907107, the zinc ion is preferably used. From the viewpoint of the above, the 疋 of the present invention is less than or equal to 0.5 wt%. From the ~ 〇. 5 (four), more material ^ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ Further, it is preferable that the present invention is a value obtained by determining the amount of zinc in the dissolved amount of the zinc ion concentration of the surface agent of the present invention, which is obtained from the compound of the upper and the sub-components. . - It is prepared by dividing the total amount of the surface treatment agent and the compound and sugar alcohol. In order to improve the film formation property of the surface of the base material of the present steel or the copper alloy, it is necessary to increase the film formation property of the surface of the base steel of the steel or the copper alloy. Copper ions may be contained in the inclusion agent. The surface of this volume has a cover = 3::: plus: If necessary, it may contain copper or if it is included, the hard and surface treatment is applied to the copper circuit part of the printed wiring board. The copper gold is a metal other than copper including copper of 50 wt% or more and tin, gold, silver, aluminum or the like of 5 or less. When the surface treatment agent of the present invention is applied to a substrate, the surface treatment agent
200907107 溫度通常只要是25〜35 例如可以藉由浸漬法、嘴霧法U用之表面處理齊 時，基材在本發明 :用於基材。採用浸潰法 15M20秒左右即可表面處理劑中浸潰的時間例如只要為 例如使用自動處理^等 用於基材時，例如可以 將本發月之表面處理劑 混合成預定組成後供給裳置的J表劑之全部成分 給裝置，在裝㈣ ^，或者將各齡分別供 等。採用後—種方口上f各成分形成财组成的方法 例如，向^ I ▲丨各成分㈣度沒有翻限定。 酸或水將其稀釋的各成分，在裝置内可以使用 接下來，基於實施例來進一步詳細 發明並不只限於這些實施例。 仁本 實施例1〜7及比較例i〜9 、將表1所示的咪唑化合物(imidazo〗e)、糖醇以及作為 生成鋅離子的化合物的鋅化合物溶解於25〇c的酸和離子 交換水的混合溶液中，使形成表〗所示的組成，得到表面 處理劑。 另一方面’準備在環氧玻璃鋼基材[日立化成工業(株) 製’品號為GEA-67N，厚度為1.6 mm]的單面貼附有18 μηι 厚的銅箔的單面貼銅的基材，在其上形成40個0.3 mm 長、8 mm寬的矩形導體圖案，製作處理用基材。將該處 理用基材浸在微蝕刻劑[MEC (株)製，商品名：MECBRITE CB-801]中，將銅箔表面僅腐蝕1 μπι，進行水洗。接下來， 12 200907107 將一塊上述基材在液溫為3〇〇c的上述所得的表面處理劑 中各浸潰60秒，進行水洗、乾燥。 在上述基材之各導體圖案上的中央部分印刷錫膏 (SOLDER COAT (株)製，品號：TAS65〇 S1_1/M9 5)， 使形成且牷為〇‘4mm、厚度為1〇〇μιη的圓形印刷圖案，200907107 The temperature is usually 25 to 35. For example, the surface can be treated by the dipping method or the nozzle method, and the substrate is used in the present invention: for the substrate. When the surface treatment agent is impregnated by the dipping method for about 15 seconds, for example, when it is used for a substrate, for example, using an automatic treatment, for example, the surface treatment agent of the present month can be mixed into a predetermined composition and then supplied to the skirt. The entire composition of the J agent is given to the device, in the (4) ^, or each age is given separately. A method of forming a financial component by using each component of the rear-side square, for example, is not limited to the degree of each component (four) of ^ I ▲ 。. The components which are diluted with acid or water can be used in the apparatus. Next, further detailed invention based on the examples is not limited to these examples. In Examples 1 to 7 and Comparative Examples i to 9 of the present invention, the imidazole compound (imidazo e) shown in Table 1, the sugar alcohol, and the zinc compound as a compound for generating zinc ions were dissolved in 25 〇c acid and ion exchange. In the mixed solution of water, the composition shown in the Table is formed to obtain a surface treatment agent. On the other hand, 'single-sided copper with a copper foil of 18 μηι thick is attached to one side of a epoxidized FRP substrate [product number: GEA-67N, thickness: 1.6 mm] The substrate was formed with 40 rectangular conductor patterns of 0.3 mm length and 8 mm width to form a substrate for processing. The substrate for the treatment was immersed in a microetching agent (MEC BRITE CB-801, manufactured by MEC Co., Ltd.), and the surface of the copper foil was only corroded at 1 μm and washed with water. Next, 12 200907107 One piece of the above substrate was immersed in the above-mentioned surface treatment agent having a liquid temperature of 3 〇〇c for 60 seconds, washed with water, and dried. A solder paste (product number: TAS65〇S1_1/M9 5, manufactured by SOLDER COAT Co., Ltd.) was printed on the central portion of each of the conductor patterns of the substrate to form a crucible of 4 mm and a thickness of 1 μm. Circular print pattern,
St熱，圈型回流焊爐中加熱印刷的基材秒:使 基材表面溫度達到V优 f ϋ 13 200907107 表1 實施例 .t谦 例編號 表面處理劑的組成(wt°/〇) 焊錫 雛 長度 (cm) 味峻化合物 糖醇 鋅化合物 [鋅離子] 溶劑 酸 離子交 換水 1 2-(1-萘甲基)苯並咪 嗤(0.2) 山梨醇 (0.5) 醋酸鋅(0.3) [0.11] 90%醋酸 (15) 餘量 1.79 2 2-(1-萘曱基)苯並咪 嗤(0.2) 山梨醇 (0_5) 醋酸鋅(0.5) [0.18] 90%醋酸 (15) 餘量 1.91 3 2-(1-萘甲基)苯並咪 嗤(0.2) 山梨醇 (0.5) 醋酸鋅(0.8) [0.29] 90%醋酸 (15) 餘量 2.15 4 2-(1-萘甲基)苯並"米 。坐(0.2) 山梨醇 (0.5) 醋酸鋅(1.0) [0.36] 90%醋酸 (15) 餘量 2.52 5 2-(1-萘甲基)苯並咪 雖2) 山梨醇 (0_5) 醋酸鋅(1.2) [0.43] 90〇/適酸 (15) 餘量 2.52 6 2-(5’-苯基)戊基苯並 咪嗤(0.2) 醇 (0.5) 醋酸辞(1_0) 阶36] 90%醋酸 (13) 餘量 2.32 7 2-苯乙基苯並咪唑 (0_2) 醇 (0.5) 甲酸辞(1.0) [0.42] 甲酸(12) 餘量 1.92 比較 例 1 2-(1-萘甲基)苯並咪 唾(0.2) 無 醋酸辞(1.0) [036] 90%醋酸 (15) 餘量 1.51 2 2-(1-萘甲基)笨並味 嗤(0.2) 山梨醇 (0.5) 無 90%醋酸 (25) 餘量 1.43 3 2-(1-萘甲基)笨並味 嗤(0.2) 無 無 90%醋酸 (25) 餘量 1.12 4 2-(5’-苯基)戊基苯並 咪嗤(0.2) 無 醋酸辞(1.0) [036] 90%醋酸 (13) 餘量 1.54 5 2-(5，-苯基)戊基苯並 咪吐(02) 醇 (0.5) 無 90%醋酸 (13) 餘量 1.31 6 2-(5’-苯基)戊基苯並 咪嗤(0.2) 無 無 90%醋酸 (13) 餘量 1.02 7 2-苯乙基苯並咪唑 (0.2) 無 甲酸辞(1.0) Γ0.42] 甲酸(12) 餘量 1.42 8 2-苯乙基苯並咪唑 (0-2) (0.5) 無 甲酸(12) 餘量 1.36 9 2-苯乙基苯並咪唑 (0-2) 無 無 曱酸(12) 餘量 1.02 由表1所示的結果可知：使用實施例1〜7所得的表面 14 200907107 ，理劑時’與比較例1〜9相比焊錫容易擴散。由此可知： 實施例1〜7所得的表面處理_觸顧擴 。 實施例8〜12及比較例1〇 八 在環氧玻璃鋼基材[日立化成工業（株）製，品番： GEA-67N ’厚度：1.6 mm]的兩面貼附18 _厚的°銅羯， 得到兩面貼銅的層合板(長·· 7·8 em，寬：4 g咖）。在該層 合板上形成_個直徑為〇.8麵的通孔，製作處理用基 材。 將該處理用基材浸在微蝕刻劑[M^C(株)製，商品名： MECBRITECB-謝）中，將銅落表面僅腐麵} μιη，進行水 洗’之後將該處理用基材各一塊分別在各實施例及比較例 10得到的酿度為30 C的表面處理劑中浸潰6〇秒，進行水 洗、乾燥。 接下來’對乾燥後的各處理用基材實施1〜5次回流處 理。回流處理中使用熱風迴圈型回流焊爐，每進行一次回 肌處理將處理用基材的表面溫度調節至240〜245°C，將處 理用基材加熱4〇秒。 咖回流處理後，使用後焊(post flux)劑[(株）ASAHI化學 研九所製’品番：AGF_88〇]，藉由噴霧對各處理用基材進 行後焊處理。 後焊處理後對各處理用基材實施流動處理。流動處理 中’將處理用基材的表面溫度調節至1〇〇。(：，藉由加熱80 秒來進彳T賴處理，之後將包含96·5敗％的錫、3 #/〇的 銀及〇·5 Wt%的銅的焊錫的溫度調節至255°C，對處理用基 15 200907107 材施行雙波(double wave)處理。需要說明的是，在雔 =中使處理用基材與焊鍚接觸25秒，之後使處理二二 、焊锡分開2.5秒，並再次使處理絲材與料接觸^、 f下來，目視確認各處理用基材的共熔焊锡狀態。其 m果如表2所示。需要說明的是，在表2中「 、 St:個通孔的焊接合格的通孔的比例。焊:合格」 的通孔疋私目視觀察時焊錫完全充填在通孔内。 表2 例·比 較例 編號 ~^面處，劑的組成 咪唑化合物糖醇 鋅化細 [鋅離子] 酸 離子交 換水St hot, loop-type reflow oven heated substrate for printing seconds: the surface temperature of the substrate reaches V-f ϋ 13 200907107 Table 1 Example. tqq example number of surface treatment agent composition (wt ° / 〇) solder Length (cm) Zhanjun Compound Zinc Zinc Compound [Zinc Ion] Solvent Acid Ion Exchange Water 1 2-(1-Naphthylmethyl)benzimid (0.2) Sorbitol (0.5) Zinc Acetate (0.3) [0.11] 90% acetic acid (15) balance 1.79 2 2-(1-naphthyl fluorenyl)benzimidazole (0.2) sorbitol (0_5) zinc acetate (0.5) [0.18] 90% acetic acid (15) balance 1.91 3 2 -(1-naphthylmethyl)benzimidazole (0.2) Sorbitol (0.5) Zinc acetate (0.8) [0.29] 90% acetic acid (15) balance 2.15 4 2-(1-naphthylmethyl)benzo " ;Meter. Sit (0.2) Sorbitol (0.5) Zinc acetate (1.0) [0.36] 90% acetic acid (15) Balance 2.52 5 2-(1-Naphthylmethyl)benzim 2) Sorbitol (0_5) Zinc acetate ( 1.2) [0.43] 90〇/acid (15) balance 2.52 6 2-(5'-phenyl)pentylbenzimidazole (0.2) alcohol (0.5) acetic acid (1_0) order 36] 90% acetic acid (13) Balance 2.32 7 2-Phenylethylbenzimidazole (0-2) Alcohol (0.5) Formic acid (1.0) [0.42] Formic acid (12) Balance 1.92 Comparative Example 1 2-(1-Naphthylmethyl)benzene Sodium salination (0.2) No acetic acid (1.0) [036] 90% acetic acid (15) Balance 1.51 2 2-(1-Naphthylmethyl) cumin and om (0.2) Sorbitol (0.5) No 90% acetic acid (25) The balance 1.43 3 2-(1-naphthylmethyl) cumin miso (0.2) without 90% acetic acid (25) balance 1.12 4 2-(5'-phenyl)pentylbenzimidazole (0.2) No acetic acid (1.0) [036] 90% acetic acid (13) Balance 1.54 5 2-(5,-Phenyl)pentylbenzimoxime (02) Alcohol (0.5) No 90% acetic acid (13) The balance of 1.31 6 2-(5'-phenyl)pentylbenzimidazole (0.2) without 90% acetic acid (13) balance 1.02 7 2-phenylethylbenzimidazole (0.2) without formic acid ( 1.0) Γ0.42] formic acid (12) balance 1.42 8 2-phenylethylbenzimidazole (0-2) (0.5) No formic acid (12) Balance 1.36 9 2-Phenylethylbenzimidazole (0-2) No decanoic acid (12) Balance 1.02 From the results shown in Table 1, the surface obtained using Examples 1 to 7 was used. 14 200907107 , when the agent is used, the solder is more likely to diffuse than the comparative examples 1 to 9. From this, it is understood that the surface treatments obtained in Examples 1 to 7 were expanded. In the examples 8 to 12 and the comparative example 1 贴, 18 _ thick ° copper enamel was attached to both surfaces of an epoxy glass reinforced plastic substrate [manufactured by Hitachi Chemical Co., Ltd., product: GEA-67N 'thickness: 1.6 mm]. Copper-clad laminates on both sides (long ······7 em, width: 4 g). On the laminate, a through hole having a diameter of 〇.8 was formed to prepare a substrate for processing. The substrate for the treatment was immersed in a microetching agent [M^C Co., Ltd., trade name: MECBRITECB-Xie), and the surface of the copper falling surface was only smeared and washed with water. One piece of the surface treatment agent having a degree of brewing of 30 C obtained in each of Examples and Comparative Example 10 was immersed for 6 sec seconds, washed with water, and dried. Next, the substrate for each treatment after drying was subjected to a reflow treatment 1 to 5 times. In the reflow treatment, a hot air loop type reflow furnace was used, and the surface temperature of the substrate for treatment was adjusted to 240 to 245 ° C for each back muscle treatment, and the substrate for treatment was heated for 4 sec. After the coffee was refluxed, a post flux agent (manufactured by ASAHI Chemical Co., Ltd.) was used for post-welding treatment of each of the substrates for processing. After the post-welding treatment, each processing substrate was subjected to a flow treatment. In the flow treatment, the surface temperature of the substrate for processing was adjusted to 1 Torr. (:, by heating for 80 seconds, the temperature of the solder containing 96.5% of the tin, 3#/〇 of the silver, and 55 Wt% of the copper was adjusted to 255 ° C, Double-wave treatment is applied to the processing substrate 15 200907107. It should be noted that the processing substrate is brought into contact with the soldering iron for 25 seconds in 雔=, and then the processing is performed for two seconds, the solder is separated for 2.5 seconds, and again The treated wire was brought into contact with the material, and the eutectic solder state of each of the processing substrates was visually confirmed. The results are shown in Table 2. In addition, in Table 2, ", St: one through hole The proportion of the through holes that are qualified for soldering. The soldering is qualified. The through holes are completely filled in the through holes when visually observed. Table 2 Example·Comparative Example No.~^ Surface, composition of the imidazole compound Fine [zinc ion] acid ion exchange water
9 VI-萘甲勒 笨並味唾(0·2) 萘甲基） 苯並啼娜2) 萘甲基） 苯並味唾((Χ2) 萘甲基） 苯並蜂峻(〇_2) 甲基） 笨並口糸口細2) 萘甲基 ） 笨並♦細 山梨醇 .(0-5) liii. Ι〇·52_ Sf^lKO.3) [0-11] mmK〇-5) [0.18] 醋酸辦0.8) [029] 醋崎1.0) [0.36] mmm2) [0.43] 90%醋 敏：15) 9〇%m 酸(15) rnif 酸(15) 90%醋 酸(15) 9〇fy〇m 瞰15) 90%醋 呶15) 69.7 793 11Ξ_ tbfe例 10 i〇^_ 山梨醇 j〇.5)_ 山梨醇 氣 山梨醇 (0.5) 100 100 100 48 91 100 100 92 - ^ ^ I____ … ，上 由表2所tf的結果可知：無較例1()相 ~12+格率高。認為這是由於覆膜中所二:雜 =化由因，在共溶焊錫時由加熱弓|起的銅表:的氧: 後也能夠維:二接:據實施例8〜12 ’即使在高温處理 由以上結果可知：使用本發明之表面處人 銅摘合金的基材的表面時，該覆膜中所含的鋅比銅^ 16 200907107 化，因此在長她管形成有魏絲 焊錫時可以抑制銅或鋼合金因加熱而氧化共您 理後也能夠維持高焊錫潤濕性。 吏在鬲溫處 另外’㈣在覆财職味錢合物鱗的錯 此發揮共炫烊錫性協同(synergism)提高的效果。曰°， 因此，使用本發明之表面處理劑 Γ 理後也能夠在包含鋼或銅合金的基材上形成^ =處 性的防銹覆膜。 孖上域具间坏錫潤濕 ，然本發明已以較佳實施例揭露如上，然其並非用以 =本發明’任何熟f此技藝者，在不脫離本發明之精神 内’當可作些許之更動與潤飾，因此本發明之保護 幸:圍备視_之申請專利範_界定者為準。 【圖式簡單說明】 無。 【主要元件符號說明】 無。 179 VI-naphthyl sulphate and saliva (0·2) naphthylmethyl) benzoxina 2) naphthylmethyl) benzo-flavored salicyl ((Χ2) naphthylmethyl) benzoxanthene (〇_2) Methyl) Stupid and mouthwash fine 2) Naphthylmethyl) Stupid and ♦ fine sorbitol. (0-5) liii. Ι〇·52_ Sf^lKO.3) [0-11] mmK〇-5) [0.18 ] acetic acid office 0.8) [029] vinegar 1.0) [0.36] mmm2) [0.43] 90% vinegar sensitive: 15) 9〇%m acid (15) rnif acid (15) 90% acetic acid (15) 9〇fy〇 m VIEW 15) 90% vinegar 呶 15) 69.7 793 11Ξ_ tbfe Example 10 i〇^_ Sorbitol j〇.5)_ Sorbitol sorbitol (0.5) 100 100 100 48 91 100 100 92 - ^ ^ I____ ... , From the results of tf in Table 2, it can be seen that there is no case 1 () phase ~ 12 + grid rate is high. It is considered that this is due to the two in the film: the impurity = the cause of the copper in the co-solubilized solder by the heating bow: the oxygen: after the dimension can also be: two: according to the embodiment 8~12 'even in From the above results, it can be seen from the above results that when the surface of the substrate of the human copper-extracted alloy on the surface of the present invention is used, the zinc contained in the film is more than that of the copper, so that when the long tube is formed with the Wei wire solder, It can suppress the wettability of copper or steel alloy by maintaining oxidation and heating.吏 鬲 鬲 另外 另外 ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ ’ Therefore, it is also possible to form a rust-preventing film on a substrate containing steel or a copper alloy after the surface treatment agent of the present invention is used. The invention has been described as a preferred embodiment of the present invention. However, it is not intended to be used in the spirit of the present invention. A few changes and retouching, so the protection of the present invention is fortunate: the definition of the application patent is based on the definition. [Simple description of the diagram] None. [Main component symbol description] None. 17
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| CN105880432A (en) * | 2016-03-31 | 2016-08-24 | 常州易藤电气有限公司 | Preparation method of copper-magnesium alloy stranded wire used for hot-tinned railway |
| CN105750354A (en) * | 2016-03-31 | 2016-07-13 | 常州易藤电气有限公司 | Method for manufacturing copper-magnesium alloy stranded wire for cold tinned railway |
| JP6402134B2 (en) * | 2016-05-12 | 2018-10-10 | 株式会社タムラ製作所 | Water-soluble preflux and surface treatment method using the same |
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| JP2561150B2 (en) * | 1989-06-09 | 1996-12-04 | 四国化成工業株式会社 | Surface treatment method for copper and copper alloys |
| JP2972295B2 (en) * | 1990-08-10 | 1999-11-08 | 四国化成工業株式会社 | Copper and copper alloy surface treatment method |
| JP2834884B2 (en) * | 1990-10-29 | 1998-12-14 | 四国化成工業株式会社 | Copper and copper alloy surface treatment method |
| JPH05163585A (en) * | 1991-12-12 | 1993-06-29 | Shikoku Chem Corp | Surface treatment of copper and copper alloy |
| JPH05237688A (en) | 1992-02-28 | 1993-09-17 | Shikoku Chem Corp | Flux composition for soldering |
| JP2923596B2 (en) | 1993-08-11 | 1999-07-26 | メック株式会社 | Surface treatment agent for copper and copper alloys using imidazole compounds |
| US5747623A (en) * | 1994-10-14 | 1998-05-05 | Tonen Corporation | Method and composition for forming ceramics and article coated with the ceramics |
| JPH09316649A (en) * | 1996-05-27 | 1997-12-09 | Matsushita Electric Ind Co Ltd | Electroless plating solution |
| JPH10251867A (en) * | 1997-03-07 | 1998-09-22 | Shikoku Chem Corp | Surface treating agent for copper and copper alloy |
| JPH11177218A (en) | 1997-12-12 | 1999-07-02 | Tamura Kaken Co Ltd | Component equipped with metal surface for electronic circuit, and surface protecting agent therefor |
| JP4546163B2 (en) * | 2004-06-10 | 2010-09-15 | 四国化成工業株式会社 | Copper or copper alloy surface treatment agent and soldering method |
| JP2007115497A (en) * | 2005-10-20 | 2007-05-10 | Mitsubishi Materials Corp | Nickel-coated copper fine particle, manufacturing method of the same, conductive paste, and manufacturing method of conductive film |
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