WO2002008491A1 - Solution d'elimination de palladium et procede correspondant - Google Patents

Solution d'elimination de palladium et procede correspondant Download PDF

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Publication number
WO2002008491A1
WO2002008491A1 PCT/JP2001/006334 JP0106334W WO0208491A1 WO 2002008491 A1 WO2002008491 A1 WO 2002008491A1 JP 0106334 W JP0106334 W JP 0106334W WO 0208491 A1 WO0208491 A1 WO 0208491A1
Authority
WO
WIPO (PCT)
Prior art keywords
palladium
nitrate
alcohol
solution according
removing solution
Prior art date
Application number
PCT/JP2001/006334
Other languages
English (en)
Japanese (ja)
Inventor
Osamu Kondo
Yoshihiro Watanabe
Fukusaburo Ishihara
Teruhiko Imai
Original Assignee
Mitsubishi Gas Chemical Company, Inc.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Mitsubishi Gas Chemical Company, Inc. filed Critical Mitsubishi Gas Chemical Company, Inc.
Priority to KR1020037000582A priority Critical patent/KR100761608B1/ko
Priority to JP2002513968A priority patent/JP4649817B2/ja
Publication of WO2002008491A1 publication Critical patent/WO2002008491A1/fr

Links

Classifications

    • 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
    • H05K3/26—Cleaning or polishing of the conductive pattern
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/30—Acidic compositions for etching other metallic material
    • 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
    • H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
    • H05K2201/07—Electric details
    • H05K2201/0753—Insulation
    • H05K2201/0761—Insulation resistance, e.g. of the surface of the PCB between the conductors
    • 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
    • H05K2203/07—Treatments involving liquids, e.g. plating, rinsing
    • H05K2203/0779—Treatments involving liquids, e.g. plating, rinsing characterised by the specific liquids involved
    • H05K2203/0786—Using an aqueous solution, e.g. for cleaning or during drilling of holes
    • H05K2203/0789—Aqueous acid solution, e.g. for cleaning or etching
    • 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
    • H05K2203/121—Metallo-organic compounds
    • 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
    • H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
    • H05K3/18—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material
    • H05K3/181—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material by electroless plating

Definitions

  • the present invention relates to a palladium removing solution and a method for removing palladium using the removing solution, and more particularly, to removing palladium present on the surface of a substrate to be treated without damaging the substrate to be treated. It concerns liquids and removal methods. Background technology ''
  • An additive method is one of the circuit pattern forming methods.
  • this additive method after palladium is applied to the entire surface of the insulating and green substrate, a copper plating layer is formed on the palladium layer by an electroless copper plating method. Only the portion of the copper-plated layer that will become the circuit pattern is covered with an etching resist, and then the copper that is not covered with the resist is removed by etching. After that, the etching resist is removed to form a circuit pattern.
  • the surface of the insulating substrate appears after the circuit pattern is formed, but the palladium remains on the surface of the insulating substrate.
  • Palladium acts as a catalyst during electroless plating, and is effective in easily forming a conductor layer.However, since it is difficult to dissolve in an ordinary etching solution, it remains after the above-described copper etching, and the circuit pattern is reduced. Decreases insulation.
  • the entire surface of the circuit pattern or the pad portion for joining the components may be subjected to electroless plating such as electroless plating or electroless plating.However, if palladium remains on the surface of the insulating substrate, However, this palladium acts as a catalyst, and nickel and gold adhere to unneeded portions, thereby deteriorating the insulation of the circuit pattern.
  • Iodine In the method of immersion in Z-ammonium iodide solution, copper dissolves simultaneously with the dissolution of palladium, so that thinning and disconnection of the wiring are likely to occur.
  • a substrate is immersed in a potassium permanganate solution, and then ultrasonically washed as required. Further, there is disclosed a method of removing palladium by immersion in a solution containing an aromatic nitro compound, an amine compound, an aminocarboxylic acid, a carboxylic acid, sodium hydroxide, and hydroxyammonium sulfate.
  • these removal solutions remove the palladium together with the resin oxide layer on the substrate surface, not only the surface of the substrate is roughened by the permanganic acid-based realm solution, but also the interface between the copper circuit pattern and the substrate is eroded. Have various disadvantages. Disclosure of the invention
  • An object of the present invention is to provide a removing solution and a removing method for removing palladium present on a surface of a substrate to be processed, which solves the above-mentioned problem, without damaging the substrate to be processed. More specifically, an object of the present invention is to easily remove palladium remaining on the surface of an insulating substrate after forming a circuit pattern in a circuit board manufacturing process. It is an object of the present invention to provide a palladium removing solution that does not corrode a wiring material, an insulating substrate, and the like, and a removing method using the removing solution.
  • the present inventors have conducted intensive studies to achieve the above object, and have found that (a) nitrate, (b) a solubilizing agent for solubilizing palladium oxide, (c) water, and if necessary, (d) The solution comprising the wetting agent and / or the chelating agent can easily remove palladium remaining on the surface of the insulating substrate after the circuit pattern is formed by the additive method in a short time, improving the insulation of the circuit pattern, They found that a highly reliable printed wiring board could be manufactured, and based on this finding, completed the present invention.
  • a first aspect of the present invention is a palladium removing solution comprising (a) a nitrate, (b) a solubilizing agent for solubilizing palladium oxide, and (c) water.
  • the removal solution may contain, if necessary, (d) a wetting agent and Z or (e) a printing agent.
  • a palladium layer is formed by attaching palladium to the surface of an insulating substrate, a copper plating layer is formed on the palladium layer, a resist is applied to the plating layer, and then etching is performed.
  • This is a palladium removal method in which palladium remaining on the substrate surface is removed using the palladium removal solution after a pattern is formed and the resist is stripped.
  • FIGS. 1A to 1D are schematic views showing a manufacturing process up to a circuit pattern forming substrate treated with the palladium removing solution of the present invention in manufacturing a printed wiring board.
  • Examples of the (a) nitrate include ammonium nitrate, lithium nitrate, zinc nitrate, manganese nitrate, nickel nitrate, cobalt nitrate, sodium nitrate, and potassium nitrate, with ammonium nitrate being particularly preferred.
  • Nitrates have the effect of oxidizing palladium.
  • the concentration of the nitrate in the palladium removing solution is from 0.001 to 40% by weight, preferably from 0.005 to 30% by weight.
  • the substance (water-solubilizing agent) for solubilizing palladium oxide (b) includes inorganic acids and salts thereof, and is preferably hydrochloric acid, nitric acid, sulfuric acid, ammonium chloride, chloride, or the like. Hydrochloride such as aluminum, sulfate such as ammonium sulfate, aluminum sulfate and the like can be mentioned.
  • the concentration of the solubilizer in the palladium-removing solution is from 0.01 to 50% by weight, preferably from 0.05 to 30% by weight.
  • other palladium oxidizing substances are mixed to increase the oxidizing power, or other palladium oxide is solubilized to increase the ability to solubilize palladium oxide.
  • the substances may be mixed.
  • the palladium removing solution of the present invention may further contain a wetting agent (d) in addition to the components (a) to (c).
  • a wetting agent (d) include surfactants, alcohols, and ethers.
  • surfactants include cationic, non-ionic, and anionic surfactants.
  • alcohols include ethyl alcohol, isopropyl alcohol, butanol, ethylene glycol, diethylene glycol, propylene glycol, and dipropylene glycol.
  • ethers ethylene glycolone monoethylene glycol, ethylene glycolone monobutylene glycol, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ethyl ether, propylene glycol monomethyl alcohol, propylene glycol alcohol Monoethynoleate propylene, propylene glycol-uremonobutyl ethenolate, dipropyleneglycore monomethinole 1-tenore, dipropyrene nicole / lemonoethynooleatenore, dipropylene darico oleno monobutynolate Diethylene glycolo resin methyl ether, dipropylene glycol resin methyl ether, polyoxyethylene methyl phenyl ether, polyoxyethylene etino Hue Nino Les ether Honoré, polyoxyethylene O Chi Roh reflex Eni Honoré ether Honoré, poly Okishiechiren'no phenyl ether and
  • the above wetting agents can be used alone or in combination of two or more.
  • concentration of palladium removing solution in the wetting agent 0s. 0 0 1-1 0 weight 0/0, preferably 0.0 0 5-5 wt%, particularly preferably 0.0 0 5 to 1 wt% .
  • the palladium removing solution of the present invention may further contain a chelating agent (e) in addition to the components ( a ) to ( c ) or the components ( a ) to (d).
  • a chelating agent is a compound that forms a complex with palladium, such as dimethyldalioxime, thiourea, thioxin (8-mercaptoquinoline), dithizone, 2-nitrosone naphthol, and p-trosodimethyla-line. Is mentioned. Dimethyl daroxime Urea is particularly preferred.
  • the chelating agent (e) not only acts as a water-solubilizing agent for the palladium oxide, but also forms a complex with a small amount of palladium that remains in the roughened surface of the insulating substrate, forming a palladium after the circuit pattern is formed. Inactive against electroless nickel plating, electroless gold plating, etc., to prevent nickel and gold from adhering to unnecessary parts and deteriorating circuit pattern insulation.
  • the concentration of the chelating agent in the palladium-removing solution is 0.01 to 5% by weight, preferably 0.01 to 2% by weight, particularly preferably 0.05 to 2% by weight. / 0 .
  • the palladium-removing solution of the present invention is an aqueous solution comprising the above-mentioned nitrate, a solubilizing agent, an optional wetting agent and Z or a chelating agent, and the balance of water. May be suspended overnight, but is usually an aqueous solution.
  • the palladium-removing solution of the present invention is produced by dissolving, dispersing, or suspending the components (a) to (b) and the optional components (d) and Z or (e) in water.
  • the order of adding each component is not particularly limited.
  • the method for removing palladium of the present invention is usually carried out by immersing the substrate to be treated in a palladium removing solution at room temperature to 80 ° C. for 1 to 10 minutes.
  • the pH of the palladium removing solution is usually used in the range of 0 to 5.
  • the pH is adjusted by changing the amount of the inorganic acid used as the component (b).
  • the used amount of the palladium removing liquid is an amount that effectively removes palladium from the substrate to be processed, and can be easily determined by those skilled in the art.
  • palladium removal method of the present invention palladium remaining after the formation of a circuit pattern can be substantially completely removed (the concentration of palladium remaining on the circuit board is 5 ppm or less).
  • FIG. 1 shows the steps up to the formation of a circuit pattern in the manufacture of a circuit board.
  • FIG. 1a shows a state in which a palladium catalyst layer 2 is formed on an insulating substrate 1. This palladium usually exists in an extremely thin layer in a state of being adsorbed on an insulating substrate, and functions as a catalyst in the case of electroless plating.
  • a conductor layer 3 consisting of a copper plating layer by electroless plating is formed as shown in Fig. 1b. It may be a conductor layer formed by applying electric plating to the attached surface as necessary.
  • the portion of the conductor layer 3 that is to be a circuit is covered with a photoresist layer 4, and then the uncovered portion of the conductor layer 3 is dissolved and removed with an etchant.
  • a photoresist layer 4 for example, a dry photo film, a photoresist ink, a screen printing resist, or the like can be used.
  • etching solution a mixed solution of sulfuric acid and hydrogen peroxide, a cupric chloride-containing solution, a ferric chloride Liquids and the like can be used.
  • a conductive circuit 3a is formed on the surface of the insulating substrate 1 as shown in FIG. 1d.
  • the palladium 2a attached to the surface of the insulating substrate 1 is not removed and remains as it is adsorbed on the insulating resin.
  • the above-mentioned palladium residual circuit board was immersed in a predetermined condition using a palladium removing solution shown in Table 1, then rinsed with pure water and dried. After that, measure the insulation resistance value of the circuit part where the circuit interval is 20 microns, measure the residual amount of palladium on the surface of the insulating substrate by X-ray fluorescence analysis and X-ray microanalyzer, and electroless nickel plating on the circuit pattern part In the test, the presence or absence of nickel on the surface of the insulating substrate and the corrosiveness of copper in the circuit pattern were observed. The measurement results and the observation results were evaluated according to the following criteria. Table 1 shows the results.
  • Solubilizing agent Combination agent 7 kinds concentration concentration concentration concentration concentration concentration concentration concentration
  • Example 7 was carried out in the same manner as in Example 7 except that a palladium removing solution having the composition shown in Table 3 was used. The experimental results are shown in Table 2. Table 2
  • Example 7 was carried out in the same manner as in Example 7, except that a palladium removing solution containing a chelating agent was used. Table 3 shows the results. Table 3
  • the palladium removing solution of the present invention is particularly It is suitable for removing palladium remaining on the surface of a flexible substrate, does not erode copper wiring, and does not roughen the surface of an insulating substrate, thereby improving the insulation of a circuit pattern. be able to.
  • the palladium on the surface is removed, so that the deterioration of insulation due to the adherence to the surface of the insulating substrate is reduced. It can be prevented beforehand.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Manufacturing Of Printed Wiring (AREA)

Abstract

L'invention concerne une solution d'élimination de palladium caractérisée en ce qu'elle renferme (a) un sel d'acide nitrique, (b) un agent qui rend les oxydes de palladium solubles dans l'eau, et (c) de l'eau. Ladite solution peut contenir, en outre, (d) une solution de mouillage et/ou (e) un agent chélatant. On peut utiliser cette solution pour éliminer le palladium de la surface d'un substrat d'isolation et accroître ainsi l'efficacité d'un tracé de circuit sans éroder un câblage en cuivre ou dégrossir la surface du substrat d'isolation.
PCT/JP2001/006334 2000-07-26 2001-07-23 Solution d'elimination de palladium et procede correspondant WO2002008491A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
KR1020037000582A KR100761608B1 (ko) 2000-07-26 2001-07-23 팔라듐 제거액 및 팔라듐 제거방법
JP2002513968A JP4649817B2 (ja) 2000-07-26 2001-07-23 パラジウム除去液およびパジジウムの除去方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2000-225938 2000-07-26
JP2000225938 2000-07-26

Publications (1)

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WO2002008491A1 true WO2002008491A1 (fr) 2002-01-31

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PCT/JP2001/006334 WO2002008491A1 (fr) 2000-07-26 2001-07-23 Solution d'elimination de palladium et procede correspondant

Country Status (4)

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JP (1) JP4649817B2 (fr)
KR (1) KR100761608B1 (fr)
TW (1) TW539773B (fr)
WO (1) WO2002008491A1 (fr)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003066795A1 (fr) * 2002-02-08 2003-08-14 Sk Corporation Agent de nettoyage et procede de nettoyage de tuyaux de chauffage
WO2004102393A1 (fr) * 2003-05-19 2004-11-25 Intellirad Solutions Pty Ltd Controle d'acces a des enregistrements medicaux
JP2008106354A (ja) * 2006-09-25 2008-05-08 Mec Kk 金属除去液及びこれを用いた金属除去方法
WO2008111389A1 (fr) * 2007-03-12 2008-09-18 Mitsubishi Chemical Corporation Solution de gravure et procédé de gravure
JP2011014924A (ja) * 2010-09-22 2011-01-20 Hitachi Metals Ltd 窒化珪素基板
CN102191501A (zh) * 2010-03-10 2011-09-21 比亚迪股份有限公司 一种钯去除液及其制备方法、一种塑料表面活化方法
CN103249254A (zh) * 2013-04-22 2013-08-14 胜宏科技（惠州）股份有限公司 一种pcb非沉铜孔除钯方法
CN114945246A (zh) * 2022-05-11 2022-08-26 深圳市松柏实业发展有限公司 线路板的除钯工艺、非金属孔的钯钝化剂及其制备方法

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20110016418A (ko) * 2009-08-11 2011-02-17 동우 화인켐 주식회사 레지스트 박리액 조성물 및 이를 이용한 레지스트의 박리방법
CN103945654A (zh) * 2013-01-18 2014-07-23 北大方正集团有限公司 钝化线路板非金属化孔中残留钯离子的方法及此方法制备的线路板
KR20170008309A (ko) 2014-07-10 2017-01-23 오꾸노 케미칼 인더스트리즈 컴파니,리미티드 수지 도금 방법

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5112582B1 (fr) * 1970-10-17 1976-04-20
WO1982004072A1 (fr) * 1981-05-21 1982-11-25 Skowronek Jerzy Procede de depouillage chimique de placages comprenant du palladium et au moins l'un des metaux cuivre et nickel et bain destine a etre utilise pour ce procede
JPS6421020A (en) * 1987-07-15 1989-01-24 Fuji Electric Co Ltd Etching recovery method for palladium

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6030520A (en) * 1997-04-23 2000-02-29 The Regents Of The University Of California Nitrate reduction

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5112582B1 (fr) * 1970-10-17 1976-04-20
WO1982004072A1 (fr) * 1981-05-21 1982-11-25 Skowronek Jerzy Procede de depouillage chimique de placages comprenant du palladium et au moins l'un des metaux cuivre et nickel et bain destine a etre utilise pour ce procede
JPS6421020A (en) * 1987-07-15 1989-01-24 Fuji Electric Co Ltd Etching recovery method for palladium

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003066795A1 (fr) * 2002-02-08 2003-08-14 Sk Corporation Agent de nettoyage et procede de nettoyage de tuyaux de chauffage
KR100674315B1 (ko) * 2002-02-08 2007-01-24 에스케이 주식회사 가열로 튜브 세척제 및 세척방법
WO2004102393A1 (fr) * 2003-05-19 2004-11-25 Intellirad Solutions Pty Ltd Controle d'acces a des enregistrements medicaux
JP2008106354A (ja) * 2006-09-25 2008-05-08 Mec Kk 金属除去液及びこれを用いた金属除去方法
WO2008111389A1 (fr) * 2007-03-12 2008-09-18 Mitsubishi Chemical Corporation Solution de gravure et procédé de gravure
JP5304637B2 (ja) * 2007-03-12 2013-10-02 三菱化学株式会社 エッチング液及びエッチング方法
CN102191501A (zh) * 2010-03-10 2011-09-21 比亚迪股份有限公司 一种钯去除液及其制备方法、一种塑料表面活化方法
JP2011014924A (ja) * 2010-09-22 2011-01-20 Hitachi Metals Ltd 窒化珪素基板
CN103249254A (zh) * 2013-04-22 2013-08-14 胜宏科技（惠州）股份有限公司 一种pcb非沉铜孔除钯方法
CN114945246A (zh) * 2022-05-11 2022-08-26 深圳市松柏实业发展有限公司 线路板的除钯工艺、非金属孔的钯钝化剂及其制备方法

Also Published As

Publication number Publication date
KR100761608B1 (ko) 2007-09-27
KR20030015392A (ko) 2003-02-20
JP4649817B2 (ja) 2011-03-16
TW539773B (en) 2003-07-01

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