US 6,475,299 B1Granted

Conversion coating composition based on nitrogen and silicon compounds and conversion coating method using the same

AssigneesSamsung Electro-Mechanics Co., Ltd., SD Chemical Co., Ltd.

InventorsByong Ho Lee, Dek Gin Yang, Yang Je Lee, Myong Gun Chong, Jae Ok Lim, Sung Wook Chun, Min Eui Hong, Kyu Hong An

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Abstract

Disclosed are a conversion coating composition for use in the surface treatment of a PCB and a conversion coating method using the same. The composition comprises 0.1-30 vol % of sulfuric acid; 0.1-15 vol % of hydrogen peroxide; 0.01-10 wt % of an organic acid; 0.1-30 wt % of a nitrogen compound; 0.01-10 wt % of an organic silicate and/or organic titanate; and 0.1-20 wt % of a film forming auxiliary, 0.1-30 wt % of an etching rate controller, 0.1-20 wt % of a reaction promoter and/or 0.1-20 g/l of a stabilizer. This composition is applied to a PCB at 10-60° C. for 1-10 min. The conversion coating film is superb in adhesive strength, acid resistance, and adhesion and can be formed with ease.

Claims23

Dependent claims

A conversion coating composition, comprising:

based on the composition,
0.1-30% by volume of sulfuric acid;
0.1-15% by volume of hydrogen peroxide;
0.01-10% by weight of an organic acid;
0.1-30% by weight of a nitrogen compound;
0.01-10% by weight of an organic silicate and or an organic titanate;
and
at least one additive selected from the group consisting of a film forming auxiliary, an etching rate controller, a reaction promoter and a stabilizer, and
wherein the organic acid comprises at least one selected from the group consisting of (i) acetic acid, (ii) propionic acid, (iii) glycolic acid, (iv) citric acid, (v) taric acid, (vi) maleic acid, (vii) malonic acid, (viii) succinic acid, (ix) phthaic acid, (x) benzoic acid, (xi) acrylic acid, and (xii) anhydride of acetic acid, propionic acid, glycolic acid, citric acid, tartaric acid, maleic acid, malonic acid, succinic acid, phthalic acid, benzoic acid, and acrylic acid,
wherein the film forming auxiliary comprises at least one selected from the group consisting of (i) hydroquinone, (ii) resorcinol, (iii) pyrocatechol, (iv) pyrogallol, (v) derivatives of hydroquinone, resorcinol, pyrocatechol, and pyrogallol, and (vi) organic sulfur compounds, in an amount of 0.1-20% by weight, if present, based on the weight of the conversion coating composition,
wherein the etching rate controller comprises at least one selected from the group consisting of N-methyl-2-pyrrolidone, N-cyclohexyl-2-pyrrolidone, 2-pyrrolidone, dimethyl formamide, dimethyl acetamide, tetrahydrofuran, acetonitrile, dioxane, all lactate, alkyl glycolate, alkyl phosphate, ketone, alcohol, and combinations thereof, in an amount of 0.1-30% by weight, if present, based on the weight of the composition coating composition,
wherein the reaction promoter comprises at least one selected from the group consisting of ammonium peroxysulfate, sodium peroxysulfate, potassium peroxysulfate, sodium peroxymonosulfate, potassium peroxymonosulfate, nitric acid, sodium nitrate, potassium nitrate, ammonium nitrate, phosphoric acid, phosphates, ferric nitrate, ferric sulfate, ferric citrate, and mixtures thereof, in all amount of 0.1-20% by weight, if present, based on the weight of the conversion coating composition, and
wherein the stabilizer comprises a chelating agent selected from the group consisting of (i) nitrilotriacetic acid (NTA), (ii) EDTA, (iii) DPTA, and (iv) metal salts of NTA, EDTA and DPTA, in an amount of 0.1-20 g/l based on the volume of the conversion coating composition.

10 more elements

A method for forming a conversion coating film on a printed circuit board, comprising the steps of:

(a) cleaning and rinsing a copper or a copper alloy printed circuit board;
(b) applying to the printed circuit board a conversion coating composition comprising:
based on the composition,
0.1-30% by volume of sulfuric acid;
0.1-1 5% by volume of hydrogen peroxide;
0.01-10% by weight of an organic acid;
0.1-30% by weight of a nitrogen compound;
0.01-10% by weight of an organic silicate and/or an organic titanate;
and
at least one additive selected from the group consisting of a film forming auxiliary, an etching rate controller, a reaction promoter and a stabilizer, and
wherein the organic acid comprises at least one selected from the group consisting of (i) acetic acid, (ii) propionic acid, (iii) glycolic acid, (iv) citric acid, (v) tartaric acid, (vi) maleic acid, (vii) malonic acid, (viii) succinic acid, (ix) phthalic acid, (x) benzoic acid, (xi) acrylic acid, and (xii) anhydride of acetic acid, propionic acid, glycolic acid, citric acid, tartaric acid, maleic acid, malonic acid, succinic acid, phthalic acid, benzoic acid, and acrylic acid,
wherein the film forming auxiliary comprises at least one selected from the group consisting of (i) hydroquinone, (ii) resorcinol, (iii) pyrocatechol, (iv) pyrogallol, (v) derivatives of hydroquinone, resorcinol, pyrocatechol, and pyrogallol, and (vi) organic sulfur compounds, in an amount of 0.1-20% by weight, if present, based on the weight of the conversion coating composition,
wherein the etching rate controller comprises at least one selected from the group consisting of N-methyl-2-pyrrolidone, N-cyclohexyl-2-pyrrolidone, 2-pyrrolidone, dimethyl formamide, dimetlyl acetamide, tetrahydrofuran, acetonitrile, dioxane, alkyl lactate, alkyl glycolate, alkyl phosphate, ketone, alcohol, and combinations thereof, in an amount of 0.1-30% by weight, if present, based on the weight of the composition coating composition,
wherein the reaction promoter comprises at least one selected from the group consisting of ammonium peroxysulfate, sodium peroxysulfate, potassium peroxysulfate, sodium peroxymonosulfate, potassium peroxymonosulfate, nitric acid, sodium nitrate, potassium nitrate, ammonium nitrate, phosphoric acid, phosphates, ferric nitrate, ferric sulfate, ferric citrate, and mixtures thereof, in an amount of 0.1-20% by weight, if present, based on the weight of the conversion coating composition, and
wherein the stabilizer comprises a chelating agent selected from the group consisting of (i) nitrilotriacetic acid (NTA), (ii) EDTA, (iii) DPTA, and (iv) metal salts of NTA, EDTA and DPTA, in an amount of 0.1-20 g/l based on the volume of the conversion coating composition;
and
(c) cleaning and drying the printed circuit board.

14 more elements

Dependencies are inferred from the claim text.

Facts

Application: 09/612,655Filed 7 Jul 2000
Priority: KR 99-277879 Jul 1999
Granted: 5 Nov 2002
Term ends: Not estimatedThe source records don’t support an estimate.

Classification10 codes

C09D 183/02
Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing…:…
C08G 77/02
Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the…
C23C 22/10
Orthophosphates: containing oxidants
C23C 22/52
Not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates: treatment…