CN103409757A - Chemical polishing solution for environment-friendly copper product and preparation method of chemical polishing solution - Google Patents

Chemical polishing solution for environment-friendly copper product and preparation method of chemical polishing solution Download PDF

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Publication number
CN103409757A
CN103409757A CN2013103741701A CN201310374170A CN103409757A CN 103409757 A CN103409757 A CN 103409757A CN 2013103741701 A CN2013103741701 A CN 2013103741701A CN 201310374170 A CN201310374170 A CN 201310374170A CN 103409757 A CN103409757 A CN 103409757A
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work
environment
chemical polishing
polishing solution
hydrogen peroxide
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CN2013103741701A
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CN103409757B (en
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姚文娣
王胜男
王鸣山
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CNNC Tianjin Technology Development Co Ltd
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CNNC Tianjin Technology Development Co Ltd
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  • Mechanical Treatment Of Semiconductor (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a chemical polishing solution for an environment-friendly copper product and a preparation method of the chemical polishing solution. The chemical polishing solution is prepared from the components according to a certain ratio: sulfuric acid, hydrogen peroxide, ethanol, a nonionic surfactant, an organic phosphate compound, a brightener and water. The preparation method comprises the steps: (i) mixing the sulfuric acid, the ethanol and the water according to the ratio, and fully mixing to prepare a semi-finished product A; (ii) mixing the nonionic surfactant, the organic phosphate compound and the brightener according to the ratio, fully mixing, adding a mixture into the semi-finished product A after the mixture is completely dissolved, and fully mixing to prepare a semi-finished product B; and (iii) adding the hydrogen peroxide into the semi-finished product B slowly according to the ratio, and fully mixing to prepare the chemical polishing solution for the environment-friendly copper product. The chemical polishing solution is a non-chromium and nontoxic environment-friendly product, is simple in manufacturing process, is conveniently used and is good in polishing effect.

Description

A kind of environment-friendly type brass work chemical brightening solution and preparation method thereof
Technical field
The invention belongs to a kind of chemical brightening solution and preparation method thereof, be specifically related to environment-friendly type brass work chemical brightening solution and preparation method thereof of a kind of Chrome-free.
Technical background
Copper product is one of metallic substance that in non-ferrous metal, usage quantity is large, application surface is wider, and its range of application is also among constantly enlarging.Brass work is of a great variety, and application spreads all over each department of national economy.And copper product has a series of good physics, chemistry, mechanics and processing characteristics, can meet the performance requriements of the no occasions of all trades and professions such as hard-core technology, communications and transportation, building decoration, aerospace, defence and military.
In national defence, military industry, mechanical means is many based on the corrosion-resistant and consideration heat conduction aspect, and employing copper is matrix, and carries out Nickel Plating Treatment at surfaces externally and internally.
Present nickel plating technology is comprised of polishing, plating, three key links of aftertreatment.Chemical rightenning is a kind of chemical corrosion under special conditions, it is optionally to dissolve by controlling the copper material surface, make the copper material surface microscopic protrude position than its calixconcavity position optimum solvation, and reach surfacing and bright purpose, for the autocatalysis electroless plating of postorder provides good condition.Traditional copper surface with chemical polishing technology adopts acid and dichromate system more, and chemical reaction process wherein is: the acid etching-passivation of copper-viscosity diffusion.Because the dichromate height is malicious and strong carinogenicity is arranged, can cause lasting pollution to environment, China and European Union all stipulate not allow public offering sexavalence chromic salts.
Summary of the invention
The present invention proposes in order to overcome the shortcoming existed in prior art, its objective is a kind of environment-friendly type brass work chemical brightening solution and preparation method thereof is provided.
Technical scheme of the present invention is: a kind of environment-friendly type brass work chemical brightening solution comprises following component and proportioning: in 1 liter of cumulative volume, wherein:
Sulfuric acid 25~35ml
Hydrogen peroxide 100~150ml
Ethanol 30~40ml
Nonionogenic tenside 0.1~0.5ml
Organic phosphoric acid compound 50~60ml
Brightening agent 0.5~1g
Water surplus
Described nonionogenic tenside is the OP-10(alkylphenol polyoxyethylene), AEO-3(fatty alcohol and ethylene oxide condensate), the AEO-9(fatty alcohol-polyoxyethylene ether) in a kind of; Described organic phosphoric acid compound is a kind of in phytic acid, Triphosaden; Described brightening agent is a kind of in Sodium orthomolybdate, citric acid, Trisodium Citrate, Seignette salt.
A kind of preparation method of environment-friendly type brass work chemical brightening solution comprises the following steps:
(I) by above proportioning, the sulfuric acid, the second alcohol and water that by mass concentration, are 98% mix, and fully stir and make work in-process A;
(II), by above proportioning, mixes nonionogenic tenside, organic phosphoric acid compound and brightening agent, fully stirs, and after it dissolves fully, joins in work in-process A, fully stirs and makes work in-process B;
By above proportioning, the hydrogen peroxide that is 30% by mass concentration slowly joins in work in-process B (III), fully stirs and makes environment-friendly type brass work chemical brightening solution.
Chemical brightening solution of the present invention is the environmentfriendly products of Chrome-free toxicological harmless, and manufacture craft is simple, easy to use, and polishing effect is good.
Embodiment:
Below, with reference to embodiment, environment-friendly type brass work of the present invention is elaborated with chemical brightening solution and preparation method thereof:
A kind of environment-friendly type brass work is as follows with chemical brightening solution component and proportioning: the cumulative volume of take is 1 liter, comprises following component and proportioning:
Sulfuric acid 25-35ml
Hydrogen peroxide 100-150ml
Ethanol 30-40ml
Nonionogenic tenside 0.1-0.5ml
Organic phosphoric acid compound 50-60ml
Brightening agent 0.5-1g
Water surplus
Described h 2 so 4 concentration is 98%; Described hydrogen peroxide mass concentration is 30%; Described nonionogenic tenside is a kind of in OP-10, AEO-3, AEO-9; Described organic phosphoric acid compound is a kind of in phytic acid, Triphosaden; Described brightening agent is a kind of in Sodium orthomolybdate, citric acid, Trisodium Citrate, Seignette salt.
A kind of environmental protection, without the preparation method of chromium-copper chemical brightening solution, comprises the following steps:
(I) by above proportioning, the sulfuric acid, the second alcohol and water that by mass concentration, are 98% mix, and fully stir and make work in-process A;
(II), by above proportioning, mixes nonionogenic tenside, organic phosphoric acid compound and brightening agent, fully stirs, and after it dissolves fully, joins in work in-process A, fully stirs and makes work in-process B;
By above proportioning, the hydrogen peroxide that is 30% by mass concentration slowly joins in work in-process B (III), fully stirs and makes environment-friendly type brass work chemical brightening solution.
Below by embodiment, the present invention is further described.
Embodiment 1:
In 1 liter of cumulative volume, component and proportioning are as follows:
Sulfuric acid 25ml
Hydrogen peroxide 100ml
Ethanol 30ml
OP-10 0.1ml
Triphosaden 50ml
Sodium orthomolybdate 0.5g
Water surplus
The preparation method comprises the following steps:
(I) by said ratio, the sulfuric acid, the second alcohol and water that by mass concentration, are 98% mix, and fully stir and make work in-process A;
(II), by said ratio, mixes OP-10, Triphosaden and Sodium orthomolybdate, fully stirs, and after it dissolves fully, joins in work in-process A, fully stirs and makes work in-process B;
By said ratio, the hydrogen peroxide that is 30% by mass concentration slowly joins in work in-process B (III), fully stirs and makes environment-friendly type brass work chemical brightening solution.
Embodiment 2:
In 1 liter of cumulative volume, component and proportioning are as follows:
Sulfuric acid 30ml
Hydrogen peroxide 125ml
Ethanol 35ml
AEO-3 0.25ml
Phytic acid 55ml
Citric acid 0.75g
Water surplus
The preparation method comprises the following steps:
(I) by said ratio, the sulfuric acid, the second alcohol and water that by mass concentration, are 98% mix, and fully stir and make work in-process A;
(II), by said ratio, mixes AEO-3, phytic acid, citric acid, fully stirs, and after it dissolves fully, joins in work in-process A, fully stirs and makes work in-process B;
By above proportioning, the hydrogen peroxide that is 30% by mass concentration slowly joins in work in-process B (III), fully stirs and makes environment-friendly type brass work chemical brightening solution.
Embodiment 3:
In 1 liter of cumulative volume, component and proportioning are as follows:
Sulfuric acid 35ml
Hydrogen peroxide 150ml
Ethanol 40ml
AEO-9 0.5ml
Triphosaden 60ml
Trisodium Citrate 1g
Water surplus
The preparation method comprises the following steps:
(I) by said ratio, the sulfuric acid, the second alcohol and water that by mass concentration, are 98% mix, and fully stir and make work in-process A;
(II), by said ratio, mixes AEO-9, Triphosaden and Trisodium Citrate, fully stirs, and after it dissolves fully, joins in work in-process A, fully stirs and makes work in-process B;
By said ratio, the hydrogen peroxide that is 30% by mass concentration slowly joins in work in-process B (III), fully stirs and makes environment-friendly type brass work chemical brightening solution.
Using method of the present invention is as follows:
(a) polishing fluid is placed in to container, room temperature gets final product; (b) will need the brass work (workpiece) of polishing to immerse in polishing fluid, take out after slight jitter 30-80s; (c) brass work of taking-up is put into to water and clean, take out after 10-20s.
Chemical brightening solution of the present invention is the environmentfriendly products of Chrome-free toxicological harmless, and manufacture craft is simple, easy to use, and polishing effect is good.

Claims (3)

1. environment-friendly type brass work chemical brightening solution is characterized in that: comprise following component and proportioning: in 1 liter of cumulative volume, wherein:
Sulfuric acid 25~35ml
Hydrogen peroxide 100~150ml
Ethanol 30~40ml
Nonionogenic tenside 0.1~0.5ml
Organic phosphoric acid compound 50~60ml
Brightening agent 0.5~1g
Water surplus
Described nonionogenic tenside is a kind of in OP-10, AEO-3, AEO-9; Described organic phosphoric acid compound is a kind of in phytic acid, Triphosaden; Described brightening agent is a kind of in Sodium orthomolybdate, citric acid, Trisodium Citrate, Seignette salt.
2. a kind of environment-friendly type brass work chemical brightening solution according to claim 1, it is characterized in that: described h 2 so 4 concentration is 98%, described hydrogen peroxide mass concentration is 30%.
3. according to the preparation method of a kind of environment-friendly type brass work chemical brightening solution claimed in claim 1, it is characterized in that: comprise the following steps:
(I) by proportioning claimed in claim 1, the sulfuric acid, the second alcohol and water that by mass concentration, are 98% mix, and fully stir and make work in-process A;
(II), by proportioning claimed in claim 1, mixes nonionogenic tenside, organic phosphoric acid compound, brightening agent, fully stirs, and after it dissolves fully, joins in work in-process A, fully stirs and makes work in-process B;
By proportioning claimed in claim 1, the hydrogen peroxide that is 30% by mass concentration slowly joins in work in-process B (III), fully stirs and makes environment-friendly type brass work chemical brightening solution.
CN201310374170.1A 2013-08-26 2013-08-26 A kind of environment-friendly type brass work chemical brightening solution and preparation method thereof Active CN103409757B (en)

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CN103409757B CN103409757B (en) 2016-01-20

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104451692A (en) * 2014-12-05 2015-03-25 贵州振华群英电器有限公司 Copper or copper alloy chemical polishing liquid and preparation method thereof
CN108624237A (en) * 2017-03-21 2018-10-09 上海铝通化学科技有限公司 A kind of Chemical Millering Polishing liquid and abrasive polishing method
CN111185596A (en) * 2020-01-06 2020-05-22 河南师范大学 Method for improving surface quality of nickel-tungsten alloy base band

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1164347A (en) * 1967-08-02 1969-09-17 Mitsubishi Edogawa Kagaku Kk A Method for Chemically Polishing Copper or Copper Alloy.
CN1340583A (en) * 2000-08-24 2002-03-20 不二见株式会社 Polishing composition and polishing method for its use
CN1382305A (en) * 1999-07-19 2002-11-27 联合讯号公司 Compositions and processes for spin etch planarization
CN1626600A (en) * 2003-11-27 2005-06-15 株式会社东芝 Slurry for CMP, polishing method and method of manufacturing semiconductor device
CN101316950A (en) * 2005-09-29 2008-12-03 卡伯特微电子公司 Composition and method for enhancing pot life of hydrogen peroxide-containing cmp slurries
CN102383132A (en) * 2010-11-24 2012-03-21 温州奥洋金属表面处理有限公司 Polishing solution for processing surfaces of copper and copper alloy by replacing copper pickling process
CN102747371A (en) * 2012-07-17 2012-10-24 许泽波 Chemical polish for copper and alloy surface treatment and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1164347A (en) * 1967-08-02 1969-09-17 Mitsubishi Edogawa Kagaku Kk A Method for Chemically Polishing Copper or Copper Alloy.
CN1382305A (en) * 1999-07-19 2002-11-27 联合讯号公司 Compositions and processes for spin etch planarization
CN1340583A (en) * 2000-08-24 2002-03-20 不二见株式会社 Polishing composition and polishing method for its use
CN1626600A (en) * 2003-11-27 2005-06-15 株式会社东芝 Slurry for CMP, polishing method and method of manufacturing semiconductor device
CN101316950A (en) * 2005-09-29 2008-12-03 卡伯特微电子公司 Composition and method for enhancing pot life of hydrogen peroxide-containing cmp slurries
CN102383132A (en) * 2010-11-24 2012-03-21 温州奥洋金属表面处理有限公司 Polishing solution for processing surfaces of copper and copper alloy by replacing copper pickling process
CN102747371A (en) * 2012-07-17 2012-10-24 许泽波 Chemical polish for copper and alloy surface treatment and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104451692A (en) * 2014-12-05 2015-03-25 贵州振华群英电器有限公司 Copper or copper alloy chemical polishing liquid and preparation method thereof
CN108624237A (en) * 2017-03-21 2018-10-09 上海铝通化学科技有限公司 A kind of Chemical Millering Polishing liquid and abrasive polishing method
CN108624237B (en) * 2017-03-21 2021-01-26 上海铝通化学科技有限公司 Chemical grinding and polishing solution and grinding and polishing method
CN111185596A (en) * 2020-01-06 2020-05-22 河南师范大学 Method for improving surface quality of nickel-tungsten alloy base band

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