CN110184595A - A kind of phosphor-copper bar brightening liquid - Google Patents

A kind of phosphor-copper bar brightening liquid Download PDF

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Publication number
CN110184595A
CN110184595A CN201910577363.4A CN201910577363A CN110184595A CN 110184595 A CN110184595 A CN 110184595A CN 201910577363 A CN201910577363 A CN 201910577363A CN 110184595 A CN110184595 A CN 110184595A
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CN
China
Prior art keywords
phosphor
copper bar
acid
brightening liquid
added
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.)
Pending
Application number
CN201910577363.4A
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Chinese (zh)
Inventor
于国军
李少利
张秀德
沈斌
姚辉
王世卓
赵长忠
张清龙
王红玲
卢爱军
崔伯峰
张育秦
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.)
Jinchuan Group Co Ltd
Original Assignee
Jinchuan Group Co Ltd
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 Jinchuan Group Co Ltd filed Critical Jinchuan Group Co Ltd
Priority to CN201910577363.4A priority Critical patent/CN110184595A/en
Publication of CN110184595A publication Critical patent/CN110184595A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C22/00Chemical 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
    • C23C22/05Chemical 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
    • C23C22/06Chemical 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
    • C23C22/48Chemical 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
    • C23C22/52Treatment of copper or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/10Other heavy metals
    • C23G1/103Other heavy metals copper or alloys of copper

Abstract

The present invention relates to a kind of phosphor-copper bar brightening liquid and preparation method thereof.The present invention consists of the following mass percentage components: the water-based thickener 2%-4% after sulfuric acid 8.0%-12.0%, hydrogen peroxide 63.0%-65.0%, organic acid 6.0%-8.0%, ethylene glycol 3.0%-5.0%, benzotriazole 3.0%-5.0%, OP-10 surfactant 7.0%-9.0%, activation.The comprehensive performances such as brightening liquid oil removing of the invention, derusting, passivation can make rapidly phosphorous copper balls to be electroplated clean bright;It is nontoxic, pollution-free and can be operated at normal temperature.

Description

A kind of phosphor-copper bar brightening liquid
Technical field
The present invention relates to a kind of phosphor-copper bar brightening liquid and preparation method thereof.
Background technique
It is further stringent to the requirement of quality of coating in electroplating industry with the development of electroplating technology, crystallite phosphorus-copper anode matter The quality of amount plays very important effect to the raising of plating solution performance and electroplating quality.Crystallite phosphorus-copper anode is texture knot Structure passes through the crystallite state copper ball of controlled micro crystallization treatment process, changes the texture structure of metal, improves the fortune of crystal molecule Kinetic force and diffusivity;The anodic phosphorous copper film of crystal grain refinement adapts to PCB electroplating technology requirement copper-base surface layer in actual production It is uniformly dissolved, copper particles from getting loose phenomenon caused by being reduced to a greater extent because of copper ball dissolution unevenness, to improve the utilization of copper Rate.Reduce cupprous generation, not only improved quality of coating but also increase anode utilization rate effectively improve plating plate quality.But corrode Phenomenon is ubiquitous, it is annual therefore caused by waste of material and economic loss it is inestimable.The corrosion and protection problem of phosphorous copper balls Temperature is also gradually increasing.The first hot alkali degreasing of traditional coating protection technique, acid pickling and rust removing after washing, not only complex process, It is seriously polluted, and efficiency is extremely low, and there is also the wastes of industrial chemicals and the energy.F in some treatment fluids-, NO2-, Cr3+Etc. toxicity Ion component complicated difficult remains problem to handle.
Summary of the invention
In order to solve the problems in the prior art, the purpose of the present invention is to provide a kind of phosphor-copper bar brightening liquid of Effictive nuisancelless And preparation method thereof.
The specific technical solution of the present invention is as follows:
A kind of phosphor-copper bar brightening liquid, consists of the following mass percentage components:
Sulfuric acid 8.0%-12.0%, hydrogen peroxide 63.0%-65.0%, organic acid 6.0%-8.0%, ethylene glycol 3.0%-5.0%, three nitrogen of benzo Water-based thickener 2%-4% after azoles 3.0%-5.0%, OP-10 surfactant 7.0%-9.0%, activation;
Specifically, the organic acid is citric acid, acetic acid or 1-hydroxy ethylidene-1,1-diphosphonic acid.
A method of preparing above-mentioned phosphor-copper bar brightening liquid, comprising the following steps: quality percentage according to claim 1 Than weighing dosage of each component, hydrogen peroxide being added in bright dipped finish slot, sequentially adds organic acid, ethylene glycol, three nitrogen of benzo Azoles is slowly added to the concentrated sulfuric acid while stirring, and water-based thickener is added when temperature is down to 20-30 DEG C while stirring, obtains brightener.
The invention has the following advantages:
The comprehensive performances such as brightening liquid oil removing of the invention, derusting, passivation can make rapidly phosphorous copper balls to be electroplated clean bright;Nontoxic, It is pollution-free and can be operated at normal temperature;The preparation method of brightening liquid solves hydrogen peroxide concentration Gao Shiyi decomposition, reaction rate The problems such as being unable to control, makes that the operation is more convenient.
Using brightening liquid of the invention treated phosphor-copper bar, exquisite appearance is bright, and no peeling tail and recess etc. do not conform to Lattice product, will not chemical residue cleaning materials pollution plating system solution, influence electro-coppering product quality, phosphor-copper bar compact crystallization rule Whole, uniform small grains, segregation-free phenomenon, P elements are evenly distributed, phosphorus content deviation < 0.0030%, and when plating can express delivery shape At uniformly fine and closely woven Cu3P black film guarantees that copper ion release uniform and stable and black film are not fallen off for a long time, it is ensured that electro-coppering produces Quality.
Specific embodiment
Embodiment 1
A kind of phosphor-copper bar brightening liquid, consists of the following mass percentage components:
Sulfuric acid 8.0%, hydrogen peroxide 65%, citric acid 7.0%, ethylene glycol 5.0%, benzotriazole 4.0%, OP-10 surfactant 8.0%, the water-based thickener 3.0% after activating.
The method of above-mentioned phosphor-copper bar brightening liquid, comprising the following steps: mass percent according to claim 1 weighs Hydrogen peroxide is added in bright dipped finish slot in dosage of each component, sequentially adds organic acid, ethylene glycol, benzotriazole, slowly adds Enter the concentrated sulfuric acid while stirring, water-based thickener is added when temperature is down to 25 DEG C while stirring, obtains brightener.
Embodiment 2
A kind of phosphor-copper bar brightening liquid, consists of the following mass percentage components:
Sulfuric acid 12.0%, hydrogen peroxide 63%, acetic acid 6.0%, ethylene glycol 4.0%, benzotriazole 4.0%, OP-10 surfactant 8.0%, the water-based thickener 3.0% after activating.
The method of above-mentioned phosphor-copper bar brightening liquid, comprising the following steps: mass percent according to claim 1 weighs Hydrogen peroxide is added in bright dipped finish slot in dosage of each component, sequentially adds organic acid, ethylene glycol, benzotriazole, slowly adds Enter the concentrated sulfuric acid while stirring, water-based thickener is added when temperature is down to 28 DEG C while stirring, obtains brightener.
Embodiment 3
A kind of phosphor-copper bar brightening liquid, consists of the following mass percentage components:
Sulfuric acid 10.0%, hydrogen peroxide 64%, 1-hydroxy ethylidene-1,1-diphosphonic acid 7.0%, ethylene glycol 4.0%, benzotriazole 4.0%, OP-10 table Water-based thickener 3.0% after face activating agent 8.0%, activation.
The method of above-mentioned phosphor-copper bar brightening liquid, comprising the following steps: mass percent according to claim 1 weighs Hydrogen peroxide is added in bright dipped finish slot in dosage of each component, sequentially adds organic acid, ethylene glycol, benzotriazole, slowly adds Enter the concentrated sulfuric acid while stirring, water-based thickener is added when temperature is down to 30 DEG C while stirring, obtains brightener.

Claims (3)

1. a kind of phosphor-copper bar brightening liquid, which is characterized in that consist of the following mass percentage components: sulfuric acid 8.0%-12.0%, Hydrogen peroxide 63.0%-65.0%, organic acid 6.0%-8.0%, ethylene glycol 3.0%-5.0%, benzotriazole 3.0%-5.0%, OP-10 table Water-based thickener 2%-4% after face activating agent 7.0%-9.0%, activation.
2. a kind of phosphor-copper bar brightening liquid as described in claim 1, it is characterised in that: the organic acid be citric acid, acetic acid or 1-hydroxy ethylidene-1,1-diphosphonic acid.
3. a kind of method for preparing phosphor-copper bar brightening liquid described in claim 1, which comprises the following steps: by power Benefit require 1 described in mass percent, weigh dosage of each component, hydrogen peroxide is added in bright dipped finish slot, has sequentially added Machine acid, ethylene glycol, benzotriazole, are slowly added to the concentrated sulfuric acid while stirring, and water-based thickener is added when being down to 20-30 DEG C in temperature It stirs simultaneously, obtains brightener.
CN201910577363.4A 2019-06-28 2019-06-28 A kind of phosphor-copper bar brightening liquid Pending CN110184595A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910577363.4A CN110184595A (en) 2019-06-28 2019-06-28 A kind of phosphor-copper bar brightening liquid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910577363.4A CN110184595A (en) 2019-06-28 2019-06-28 A kind of phosphor-copper bar brightening liquid

Publications (1)

Publication Number Publication Date
CN110184595A true CN110184595A (en) 2019-08-30

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CN201910577363.4A Pending CN110184595A (en) 2019-06-28 2019-06-28 A kind of phosphor-copper bar brightening liquid

Country Status (1)

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CN (1) CN110184595A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111996575A (en) * 2020-09-08 2020-11-27 宁波江丰电子材料股份有限公司 Surface treatment method of CuP electroplating anode material

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102747371A (en) * 2012-07-17 2012-10-24 许泽波 Chemical polish for copper and alloy surface treatment and preparation method thereof
CN104388961A (en) * 2014-11-14 2015-03-04 平高集团有限公司 Copper cleaning agent and preparation method thereof
CN108411314A (en) * 2018-04-02 2018-08-17 深圳市祥盛兴科技有限公司 A kind of copper and copper alloy surface cleaning solution and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102747371A (en) * 2012-07-17 2012-10-24 许泽波 Chemical polish for copper and alloy surface treatment and preparation method thereof
CN104388961A (en) * 2014-11-14 2015-03-04 平高集团有限公司 Copper cleaning agent and preparation method thereof
CN108411314A (en) * 2018-04-02 2018-08-17 深圳市祥盛兴科技有限公司 A kind of copper and copper alloy surface cleaning solution and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
胡磊等: "新型铜及铜合金酸洗光亮剂研究", 《中国洗涤用品工业》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111996575A (en) * 2020-09-08 2020-11-27 宁波江丰电子材料股份有限公司 Surface treatment method of CuP electroplating anode material
CN111996575B (en) * 2020-09-08 2023-01-17 宁波江丰电子材料股份有限公司 Surface treatment method of CuP electroplating anode material

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Application publication date: 20190830