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WO2014064050A1 - Traitement de corps moulés contenant du cuivre avec un mélange contenant des acides exempts de chlore et de carboxyle et des agents d'oxydation - Google Patents

Traitement de corps moulés contenant du cuivre avec un mélange contenant des acides exempts de chlore et de carboxyle et des agents d'oxydation Download PDF

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Publication number
WO2014064050A1
WO2014064050A1 PCT/EP2013/071966 EP2013071966W WO2014064050A1 WO 2014064050 A1 WO2014064050 A1 WO 2014064050A1 EP 2013071966 W EP2013071966 W EP 2013071966W WO 2014064050 A1 WO2014064050 A1 WO 2014064050A1
Authority
WO
WIPO (PCT)
Prior art keywords
copper
aqueous mixture
weight
chlorine
etching
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2013/071966
Other languages
German (de)
English (en)
Inventor
Thomas PAASCHE
Henning Urch
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BASF SE
Original Assignee
BASF SE
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 BASF SE filed Critical BASF SE
Publication of WO2014064050A1 publication Critical patent/WO2014064050A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C23F1/18—Acidic compositions for etching copper or alloys thereof
    • 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
    • C23F1/46—Regeneration of etching compositions
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/10—Other heavy metals
    • C23G1/103—Other heavy metals copper or alloys of copper
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/36—Regeneration of waste pickling liquors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
    • H01L21/321—After treatment
    • H01L21/3213—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer
    • H01L21/32133—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer by chemical means only
    • H01L21/32134—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer by chemical means only by liquid etching only
    • 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
    • H05K3/02—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding
    • H05K3/06—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding the conductive material being removed chemically or electrolytically, e.g. by photo-etch process
    • H05K3/067—Etchants
    • 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

Definitions

  • the present invention relates to a process for the treatment of moldings containing copper with a mixture containing chlorine-free acids without carboxyl groups and Oxidati- onsstoff. Furthermore, the invention also relates to mixtures comprising methanesulfonic acid and hydrogen peroxide. Another object of the invention is the use of such mixtures containing chlorine-free acids without carboxyl groups and oxidizing agents, in particular methanesulfonic acid and hydrogen peroxide, for etching or pickling of moldings containing copper.
  • Copper and copper alloys are often used as conductive materials in the semiconductor manufacturing field. Copper tracks are often found to be conductive connecting elements of semiconductor structures, for example in integrated circuits on boards.
  • mixtures containing acids for example hydrochloric acid, acetic acid, sulfuric acid or nitric acid and oxidizing agents such as pereroxides, persulfates, permanganates, Fe (III) solutions, bromine or Cr (VI) compounds are frequently used.
  • acids for example hydrochloric acid, acetic acid, sulfuric acid or nitric acid and oxidizing agents such as pereroxides, persulfates, permanganates, Fe (III) solutions, bromine or Cr (VI) compounds are frequently used.
  • WO 201 1/0171 19 A2 describes wet-chemical etching processes for removing copper in the processing of semiconductors by means of solutions comprising complexing agents and oxidizing agents in a pH range from 5 to 12.
  • US 2005/0056616 A1 and US 2006/0183056 A1 describe methods for etching copper and copper alloys. With the aid of compositions containing weak and strong complexing agents for copper and oxidizing agents, the surfaces of copper or copper alloys are treated at a pH of 6 to 12.
  • US 7,465,408 B1 describes methods of etching copper-containing materials by first contacting the material with a first solution which converts a portion of the material to a passivating layer.
  • This first solution contains a peroxide, a first organic acid, and water at a pH of 2 to 6.
  • the passivating coating is contacted with a second solution to remove the passivating film, this second solution being a second contains organic acid and water.
  • copper is often deposited on an epoxy resin board.
  • a photoresist photoresist
  • a photoresist is applied and selectively exposed at certain points.
  • Unexposed residues of the photoresist are usually removed in further processing steps with alcoholic solutions.
  • aqueous mixtures of CuC, FeC or HCl and hydrogen peroxide are used as etching mixtures for removing or building structures containing copper or for pickling surfaces containing copper.
  • the resulting in these wet chemical etching mixtures contain after removal of the copper in addition to the copper ions a high proportion of chloride ions in the solution and are therefore a simple reprocessing and recovery of copper, for example by electrolysis, because of the formation of chlorine gas, difficult to access.
  • the object of the present invention was therefore to find processes for the treatment of moldings containing copper, which allow a simple reprocessing and recovery of copper after the treatment.
  • a further object of the invention was to provide wet-chemical etching processes which lead to well-defined structures in the removal of copper-containing materials, in particular to structures with smooth surfaces and defined edges.
  • populated boards contain up to 25% by weight of pure copper.
  • the layer thickness of the copper is from 20 to 45 ⁇ thick, which corresponds to about 0.02 wt .-% with an assumed total thickness of a board of 1 mm.
  • the relative content of copper thus generally increases.
  • such molded articles contain from 0.01% by weight to 50% by weight of copper, based on the total amount of molding. Particularly preferably from 0.01 to 25 wt .-%. Further preferably, the copper occurs in the form of metallic copper or copper alloys with other metals, such as molybdenum.
  • the chlorine-free acids without carboxyl groups (a.) are selected from the group of alkylsulfonic acids, tetrafluoroboric acid, sulfuric acid, hexafluorosilicic acid, trifluoroacetic acid, trifluoromethanesulfonic acid. Methanesulfonic acid is particularly preferred as chlorine-free acid without carboxyl groups (a.).
  • the oxidizing agents (b.) are selected from the group of peroxide compounds and perborate compounds, preferably from the group consisting of hydrogen peroxide, sodium perborate, barium perborate, carbamate peroxide and urea peroxide, peroxycarboxylic acids such as peramaic acid or peracetic acid. Very particular preference is given to hydrogen peroxide as oxidizing agent (b.).
  • the component (c.) Contains as an aqueous solvent from 10 to 100 wt .-% water. Preference is given to using water as the aqueous solvent (c.). In addition to water, further polar liquids such as alcohols or ionic liquids may be present in the aqueous solvent.
  • the aqueous mixture (M) may contain as additional component (d.) Additional additives.
  • Preferred additives (d.) are surfactants, complexing agents or corrosion inhibitors.
  • surfactants serve to improve the wetting of the molding or of the copper with the aqueous mixture (M). It is possible to use anionic, cationic, nonionic or amphoteric surfactants.
  • the surfactants may also be polymeric surfactants and preferably have a block structure. Surfactants are known to those skilled in the art and knowledgeable in the art and can be purchased commercially. It is preferred to use anionic or nonionic surfactants. For example, alkyl polyglycosides can be used as surfactants.
  • Complexing agents are often used to complex copper ions and thus to accelerate the dissolution process of the copper.
  • Corresponding complexing agents are known to the skilled person from the prior art and his expertise and can be purchased commercially.
  • ethylenediaminetetraacetic acid (EDTA) methylglycine diacetic acid
  • GLDA glutamic acid diacetic acid
  • NTA nitrilotriacetic acid
  • corrosion inhibitors are used in the treatment of moldings containing copper to prevent or suppress unwanted corrosion effects on materials.
  • Corresponding corrosion inhibitors are known to those skilled in the art and their knowledge and can be purchased commercially.
  • alkyl phosphates, 2-butyne-1,4-diol, propargyl alcohol, ethynylcarbinol alkoxylate, polyethylene lenimin, thiodiglycol ethoxylate can be used as corrosion inhibitors.
  • the aqueous mixture contains (M)
  • the quantities are in each case based on the total amount of components (a.), (b.), (c.) and (d.) and the sum of the amounts of all components (a.), (b.), (c. ) and (d.) is 100% by weight.
  • the mixture (M) in particular before the treatment of the shaped body, particular preference is given to containing no further components apart from the components (a.), (B.), (C.) And optionally (d.).
  • the total amount of all additives (d.) In the aqueous mixture (M) is, as described above, in the range from 0 to 10% by weight, preferably from 0 to 5% by weight, in particular from 0 to 3% by weight. -%.
  • Surfactants are preferably used in an amount of 0.5 to 2 wt .-%.
  • Complexing agents are preferably used in an amount of 0.5 to 5 wt .-%.
  • Corrosion inhibitors are preferably used in an amount of 0.1 to 1 wt .-%.
  • the aqueous mixture (M) has a pH of from -0.5 to 5, preferably from 0 to 5, particularly preferably from 0 to 3, very particularly preferably from 0 to 2, in particular from 0 to 1 ,
  • the pH of the mixture (M) is determined by glass electrode.
  • the copper contained may be distributed arbitrarily in the molding as long as it at least partially in contact with the aqueous mixture (M) or comes into contact or is brought into contact.
  • the copper contained is at least partially on at least one surface of the shaped body.
  • the molded body is a printed circuit board (board) or printed circuit board.
  • copper is usually removed from or from the shaped body, preferably metallic copper in the form of copper ions is separated from or from the shaped body.
  • the aqueous mixture (M) additionally contains dissolved copper, preferably in the form of copper ions, and the aqueous mixture is separated from the solid in a further process step. A so-called waste solution is obtained.
  • Another object of the invention is a process for working up the aqueous mixture (M), which additionally contains (e.) Dissolved copper (waste solution), wherein an electrolysis is carried out on this waste solution to at least partially deposit the dissolved copper as metallic copper.
  • Typical conditions for the electrowinning of copper on stainless steel electrodes are high current densities of 250-1000A / m 2 at 0.3-0.4V.
  • the electrode distance is 5 to 50 mm.
  • MI mixtures
  • a. From 10 to 40 wt .-% of methanesulfonic acid
  • b. From 10 to 20 wt .-%, preferably from 15 to 20
  • These mixtures can also be excellently mixed with further additives (d.)
  • additives rens for the treatment of moldings containing copper.
  • rens for the treatment of moldings containing copper As a rule, from 0 to 10% by weight of additives (d.) Are contained in the mixtures.
  • the quantities given in each case relate to the total amount of components (a.), (B.), (C.) And optional (d.) And the sum of the amounts of all components (a.), (B.), (C) , (d.) is 100% by weight.
  • these mixtures according to the invention can be used for etching or pickling of shaped bodies containing copper, wherein preferably the copper contained is at least partially located on at least one surface of the shaped body.
  • the shaped body is a circuit board.
  • the present invention provides processes for the treatment of moldings containing copper which, after treatment, allow easy reprocessing and recovery of copper. Furthermore, wet-chemical etching processes are provided which lead to well-defined structures, in particular to structures with smooth surfaces and defined edges, when removing copper-containing materials.
  • the aqueous mixture M1 was obtained by mixing the individual components with water.
  • M1 10% by weight of methanesulfonic acid (MSA), 15% by weight of H 2 O 2 , 75% by weight of H 2 O.
  • the determination of the polarization resistance was carried out in a potential range of ⁇ 5 mV against the corrosion potential (Ecorr) using a scan rate of 0.1 mV / s.
  • the measured potential (E) plotted against the current density (j) was fitted to a straight line, from the slope of the line Rp was determined.
  • the Rp value indicates the resistance of a metal to the transfer of electrons to an electroactive species in solution. Higher values of Rp mean higher corrosion resistance to uniform corrosion. Lower values thus correlate with a faster dissolution of the metal. Resolution of copper:
  • E caloric reference electrode saturated with reference cell vs. SCE
  • time or current density show the significantly increased rate of copper dissolution for M1 compared to V1.
  • the value of E for M1 is about +0.22 V while for V1 it is about -0.5 V in a period up to 60 hours.
  • the remainder to 100% by weight is water at L6 to L15.
  • the copper-coated circuit boards were placed at a temperature of 18 ° C in 100 ml of the respective solution.
  • the copper-coated circuit boards were further laid at 100 ° C. of the respective solution at a temperature of 18 ° C. for 12 to 50 minutes.

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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)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Computer Hardware Design (AREA)
  • Power Engineering (AREA)
  • ing And Chemical Polishing (AREA)

Abstract

L'invention concerne un procédé pour le traitement de corps moulés contenant du cuivre, un mélange aqueux (M) qui contient (a.) des acides exempts de chlore et sans groupes carboxyle, (b.) des agents d'oxydation, (c.) des solvants aqueux et éventuellement des additifs supplémentaires étant mis en contact avec le corps moulé. Le procédé est caractérisé, entre autres, en ce que le mélange aqueux (M) contient en outre, après le mordançage ou le décapage, du cuivre dissous et est séparé du corps solide. L'invention concerne aussi un procédé pour traiter par électrolyse le mélange aqueux (M) séparé qui contient en plus du cuivre dissous. L'invention concerne également des mélanges (MI) contenant (a.) de 10 à 40 % en poids d'acide méthanesulfonique, (b.) de 10 à 20 % en poids de peroxyde d'hydrogène et (c.) de 40 à 80 % en poids d'eau et leur utilisation pour mordancer et décaper des corps moulés contenant du cuivre.
PCT/EP2013/071966 2012-10-25 2013-10-21 Traitement de corps moulés contenant du cuivre avec un mélange contenant des acides exempts de chlore et de carboxyle et des agents d'oxydation Ceased WO2014064050A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP12189999 2012-10-25
EP12189999.1 2012-10-25

Publications (1)

Publication Number Publication Date
WO2014064050A1 true WO2014064050A1 (fr) 2014-05-01

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2013/071966 Ceased WO2014064050A1 (fr) 2012-10-25 2013-10-21 Traitement de corps moulés contenant du cuivre avec un mélange contenant des acides exempts de chlore et de carboxyle et des agents d'oxydation

Country Status (2)

Country Link
TW (1) TW201418521A (fr)
WO (1) WO2014064050A1 (fr)

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4378270A (en) * 1981-10-29 1983-03-29 Learonal, Inc. Method of etching circuit boards and recovering copper from the spent etch solutions
US4632727A (en) * 1985-08-12 1986-12-30 Psi Star Copper etching process and solution
EP0665309A1 (fr) * 1994-01-31 1995-08-02 Emil Krechen Industrievertretungen GmbH Procédé de décapage de cuivre
DE19732419A1 (de) * 1996-07-29 1998-02-05 Ebara Densan Ltd Ätzmittel, Verfahren zum Aufrauhen von Kupferoberflächen und Verfahren zum Herstellen von Leiterplatten
US20040089838A1 (en) * 1998-06-09 2004-05-13 Ebara Densan Ltd. Method for roughening copper surface
US20050056616A1 (en) 2003-09-17 2005-03-17 International Business Machines Corporation Method for isotropic etching of copper
US7465408B1 (en) 2003-12-03 2008-12-16 Advanced Micro Devices, Inc. Solutions for controlled, selective etching of copper
WO2011017119A2 (fr) 2009-08-04 2011-02-10 Novellus Systems, Inc. Procédés de gravure humide pour retrait de cuivre et planarisation dans un traitement de semi-conducteurs

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4378270A (en) * 1981-10-29 1983-03-29 Learonal, Inc. Method of etching circuit boards and recovering copper from the spent etch solutions
US4632727A (en) * 1985-08-12 1986-12-30 Psi Star Copper etching process and solution
EP0665309A1 (fr) * 1994-01-31 1995-08-02 Emil Krechen Industrievertretungen GmbH Procédé de décapage de cuivre
DE19732419A1 (de) * 1996-07-29 1998-02-05 Ebara Densan Ltd Ätzmittel, Verfahren zum Aufrauhen von Kupferoberflächen und Verfahren zum Herstellen von Leiterplatten
US20040089838A1 (en) * 1998-06-09 2004-05-13 Ebara Densan Ltd. Method for roughening copper surface
US20050056616A1 (en) 2003-09-17 2005-03-17 International Business Machines Corporation Method for isotropic etching of copper
US20060183056A1 (en) 2003-09-17 2006-08-17 International Business Machines Corporation Method for isotropic etching of copper
US7465408B1 (en) 2003-12-03 2008-12-16 Advanced Micro Devices, Inc. Solutions for controlled, selective etching of copper
WO2011017119A2 (fr) 2009-08-04 2011-02-10 Novellus Systems, Inc. Procédés de gravure humide pour retrait de cuivre et planarisation dans un traitement de semi-conducteurs

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Publication number Publication date
TW201418521A (zh) 2014-05-16

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