CN101225259A - Anticorrosion preservative used for silver layer surface - Google Patents

Anticorrosion preservative used for silver layer surface Download PDF

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Publication number
CN101225259A
CN101225259A CNA2007100728945A CN200710072894A CN101225259A CN 101225259 A CN101225259 A CN 101225259A CN A2007100728945 A CNA2007100728945 A CN A2007100728945A CN 200710072894 A CN200710072894 A CN 200710072894A CN 101225259 A CN101225259 A CN 101225259A
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Prior art keywords
solvent
silver layer
silver
layer surface
anticorrosion
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CNA2007100728945A
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Chinese (zh)
Inventor
周黎明
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Jing Wenli
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Jing Wenli
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Priority to CNA2007100728945A priority Critical patent/CN101225259A/en
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Abstract

The invention relates to a corrosion-proof protective agent used for surfaces of silver coatings, which is characterized in that: the components and contents are a film forming matter with a R1-(CH2)n-R2 structure of 0.1g to 10g/L, a solvent of 1% to 20% (V/V), a surface-active material of 0.1g to 5g/L and excess water; in the film forming matter with a R1- (CH2)n-R2 structure, R1 is phenyl, phenmethyl, hydrocarbon of alkenes and alkanes, hydrocarbon of alkynes and alkanes, hydroxyl, carboxyl, alkoxy or alkyl, and n is 8 to 20, and R2 is -COOH, -NH2, -SH, -COONH2, -S-S-R or -CN, and the corrosion-proof protective solute comprises one or more film forming matters; the solvent is alcohol solvent, ester solvent, water soluble ether solvent or polar solvent; the surface-active material is a nonionic surface-active material or a cation surface-active material. The corrosion-proof protective agent has the advantages of being beneficial to environmental protection, simple configuration and low processing cost for protecting surfaces of silver coatings.

Description

The anticorrosion preservative that is used for silver layer surface
Technical field
The surface anticorrosion and the protection that the present invention relates to argent are handled, and relate in particular to the treatment agent that generates the protection against corrosion organic protective film of one deck nanometer grade thickness at silver surface.
Background technology
Because the influence of airborne S-contained substance etc., silvering surface corrosion-vulnerable and oxidation stain causes silvering from still all being subjected to very big influence on the actual functions of use in appearance.In order to address this problem, prior art adopts technologies such as electrolysis, passivation, surperficial spray treatment usually, but there are weak points such as not environmental protection, operational difficulty and processing cost height in these processing methodes.Since the nineties in last century, begun the research of unimolecular layer nanometer organic membrane in the world, and tried out in metal surface anticorrosive and handle, but owing to do not find suitable organic membrane molecular structure, and can't solve the technical problem of preparation process and abandoned gradually.
Summary of the invention
The technical problem to be solved in the present invention is to avoid above-mentioned the deficiencies in the prior art part and proposes a kind of anticorrosion preservative that is used for silver layer surface; after being used in silver layer surface; this anticorrosion preservative can be at the silver layer surface oriented adsorption; and based on monomolecular adsorption; multilayer adsorption further takes place; thereby form the fine and close protective membrane of one deck nanometer grade thickness at silver layer surface,, and do not influence the welding property of silver layer with the influence of secluding air to silver layer surface.
The present invention solve the technical problem can be by realizing by the following technical solutions: dispose a kind of anticorrosion preservative that is used for silver layer surface, its component and content are:
Structure is filmogen 0.1g～10g/L of R1-(CH2) n-R2
Solvent 1%～20% (V/V)
Tensio-active agent 0.1g～5g/L
Water surplus
Described structure is that the filmogen R1 of R1-(CH2) n-R2 is phenyl, benzyl, alkene alkane, alkynes alkane, hydroxyl, carboxyl, alkoxyl group or alkyl, n=8～20, R 2For-COOH ,-NH 2,-SH ,-COONH 2,-S-S-R or-CN, described anticorrosion preservative comprises one or more described filmogen.
Described solvent is alcoholic solvent, contain the solvent of Ester and heterocycle material, water-soluble ethers kind solvent or polar solvent; Described alcoholic solvent can be that ethanol, butanols, Virahol, molecular weight are that 200～1000 polyoxyethylene glycol and/or molecular weight are 200～1800 polypropylene glycol; Described polar solvent is dimethyl formamide (DMF) and/or dimethyl sulfoxide (DMSO) (DMSO).
Described tensio-active agent is nonionogenic tenside or cats product.Described nonionogenic tenside can be selected the segmented copolymer of alkyl alcohol polyethenoxy ether class or ethylene oxide and propylene oxide for use.Described cats product can be selected dodecyl benzyl dimethyl ammonium chloride (1227) for use.
The present invention also comprises co-solvent, and content is 1%～10% (V/V).The optional spent glycol of this co-solvent, glycerol and/or glycol ether.
Compare with prior art, technique effect of the present invention is:
1. complete compliance with environmental protection requirements of formula material, and configuration and use do not produce environmentally harmful material;
2. formula material is stirred at normal temperatures and just can be configured to anticorrosion preservative of the present invention, configuration is simple; Use anticorrosion preservative of the present invention generally to adopt aqueous solution soaking or spray mode, convenience simple to operation;
3. use protective material of the present invention to need not specific installation and special processing mode, and because the protective layer on the silver layer is a nano level, the filmogen consumption is extremely low, thereby processing cost is cheap.
Embodiment
Below rescuing each most preferred embodiment of the present invention is described in further detail.
Below the protectant concrete preparation method of silver layer among each embodiment identical.At normal temperatures, solvent such as ethanol, polyoxyethylene glycol etc. are added in the enamel still of clean band stirring, then pure water is added to 2/3rds volume, filmogen and co-solvent such as glycerol etc. are prepared, mixed jointly in beaker, under agitation add in the stirring tank and go, dissolve fully to solid matter, add tensio-active agent such as alkyl alcohol Soxylat A 25-7 etc. then, and water complements to the volume of requirement, continue to be stirred to and mixed evenly stop to stir, leave standstill the overanxious product that promptly becomes.
Embodiment 1: the present invention is used for the protective material of silver layer surface, and its component and content are:
Benzene TETRADECONIC ACID 2g/L
Ethanol 5%
Glycerol 3%
Polyoxyethylene nonylphenol ether (OP-10) 0.6g/L
All the other pure water
Use the silver protecting agent of the embodiment of the invention 1, under following processing condition:
Join the groove ratio Treatment temp Treatment time Processing mode Post-treatment condition
100ml/L, all the other are pure water 50℃ 50 seconds Soak or spray Hot water cleans, and uses ultrasonic wave water cleaning, drying again
Detect silver layer protection effect after handling 1000 wiring boards
Deposit a week in the air Deposited in the air three months Deposited in the air six months 10％FeCl 3The solution destructive test
The silver face does not have the corrosion nondiscoloration The silver face does not have the corrosion nondiscoloration The silver face does not have the corrosion nondiscoloration Silver-colored face does not have the corrosion nondiscoloration in 30 seconds
Solderability test: through three to six reflow ovens (265 ℃ of top temperature, top 65 seconds time of temperature) baking, the no tinol of seal (tin/copper/silver alloys) is crossed reflow ovens and manual immersed solder test (265 ℃, tin/copper/silver alloys) respectively then
Embodiment 2: the present invention is used for the protective material of silver layer surface, and its component and content are:
Oxyethyl group amino dodecane 5g/L
Virahol 8%
Glycol ether 7%
1227 0.5g/L
All the other pure water
Use the silver protecting agent of the embodiment of the invention 2, under following processing condition:
Join the groove ratio Treatment temp Treatment time Processing mode Post-treatment condition
100ml/L, all the other are water 50℃ 50 seconds Soak or spray Hot water cleans, and uses ultrasonic wave water cleaning, drying again
Handle the silver layer protection effect that 1000 wiring board tests record
Deposit a week in the air Deposited in the air three months Deposited in the air six months 10％FeCl 3The solution destructive test
The silver face does not have the corrosion nondiscoloration The silver face does not have the corrosion nondiscoloration The silver face does not have the corrosion nondiscoloration Silver-colored face does not have the corrosion nondiscoloration in 30 seconds
Solderability test:, print soldering paste (tin/copper/silver alloys) then respectively and cross reflow ovens and manual immersed solder test (265 ℃, tin/copper/silver alloys) through three to six reflow ovens (265 ℃ of top temperature, top 65 seconds time of temperature) baking
Embodiment 3: the present invention is used for the protective material of silver layer surface, and its component and content are:
Stearylamide 5g/L
Virahol 8%
Glycol ether 7%
1227 0.5g/L
All the other pure water
Use the silver protecting agent of the embodiment of the invention 3, under following processing condition:
Join the groove ratio Treatment temp Treatment time Processing mode Post-treatment condition
100ml/L, all the other are water 50℃ 50 seconds Soak or spray Hot water cleans, and uses ultrasonic wave water cleaning, drying again
Handle the silver layer protection effect that 1000 wiring board tests record
Deposit a week in the air Deposited in the air three months Deposited in the air six months 10％FeCl 3The solution destructive test
The silver face does not have the corrosion nondiscoloration The silver face does not have the corrosion nondiscoloration The silver face does not have the corrosion nondiscoloration Silver-colored face does not have the corrosion nondiscoloration in 30 seconds
Solderability test:, print soldering paste (tin/copper/silver alloys) then respectively and cross reflow ovens and manual immersed solder test (265 ℃, tin/copper/silver alloys) through three to six reflow ovens (265 ℃ of top temperature, top 65 seconds time of temperature) baking
Figure A20071007289400072
Embodiment 4: the present invention is used for the protective material of silver layer surface, and its component and content are:
Allyl group Dodecyl Mercaptan 5g/L
Virahol 8%
DSMO 7％
1227 0.5g/L
All the other pure water
Use the silver protecting agent of the embodiment of the invention 4, under following processing condition:
Join the groove ratio Treatment temp Treatment time Processing mode Post-treatment condition
100ml/L, all the other are water 50℃ 50 seconds Soak or spray Hot water cleans, and uses ultrasonic wave water cleaning, drying again
Handle the silver layer protection effect that 1000 wiring board tests record
Deposit a week in the air Deposited in the air three months Deposited in the air six months 10％FeCl 3The solution destructive test
The silver face does not have the corrosion nondiscoloration The silver face does not have the corrosion nondiscoloration The silver face does not have the corrosion nondiscoloration Silver-colored face does not have the corrosion nondiscoloration in 30 seconds
Solderability test:, print soldering paste (tin/copper/silver alloys) then respectively and cross reflow ovens and manual immersed solder test (265 ℃, tin/copper/silver alloys) through three to six reflow ovens (265 ℃ of top temperature, top 65 seconds time of temperature) baking
Figure A20071007289400081
Embodiment 5: the present invention is used for the protective material of silver layer surface, and its component and content are:
Allyl group Dodecyl Mercaptan 2g/L
Oxyethyl group amino dodecane 3g/L
Virahol 8%
DMF 7％
1227 0.5g/L
All the other pure water
Use the silver protecting agent of the embodiment of the invention 5, under following processing condition:
Join the groove ratio Treatment temp Treatment time Processing mode Post-treatment condition
100ml/L, all the other are water 50℃ 50 seconds Soak or spray Hot water cleans, and uses ultrasonic wave water cleaning, drying again
Handle the silver layer protection effect that 1000 wiring board tests record
Deposit a week in the air Deposited in the air three months Deposited in the air six months 10％FeCl 3The solution destructive test
The silver face does not have the corrosion nondiscoloration The silver face does not have the corrosion nondiscoloration The silver face does not have the corrosion nondiscoloration Silver-colored face does not have the corrosion nondiscoloration in 30 seconds
Solderability test:, print soldering paste (tin/copper/silver alloys) then respectively and cross reflow ovens and manual immersed solder test (265 ℃, tin/copper/silver alloys) through three to six reflow ovens (265 ℃ of top temperature, top 65 seconds time of temperature) baking
Figure A20071007289400091
Embodiment 6: the present invention is used for the protective material of silver layer surface, and its component and content are:
Stearylamide 2g/L
Oxyethyl group amino dodecane 3g/L
Virahol 8%
DMF 7％
TX-10 (polyoxyethylene octylphenol ether) 0.5g/L
All the other pure water
Use the silver protecting agent of the embodiment of the invention 6, under processing condition once:
Join the groove ratio Treatment temp Treatment time Processing mode Post-treatment condition
100ml/L, all the other are water 50℃ 50 seconds Soak or spray Hot water cleans, and uses ultrasonic wave water cleaning, drying again
Handle the silver layer protection effect that 1000 wiring board tests record
Deposit a week in the air Deposited in the air three months Deposited in the air six months 10％FeCl 3The solution destructive test
The silver face does not have the corrosion nondiscoloration The silver face does not have the corrosion nondiscoloration The silver face does not have the corrosion nondiscoloration Silver-colored face does not have the corrosion nondiscoloration in 30 seconds
Solderability test:, print soldering paste (tin/copper/silver alloys) then respectively and cross reflow ovens and manual immersed solder test (265 ℃, tin/copper/silver alloys) through three to six reflow ovens (265 ℃ of top temperature, top 65 seconds time of temperature) baking
Figure A20071007289400092
Embodiment 7: the present invention is used for the protective material of silver layer surface, and its component and content are:
Benzene TETRADECONIC ACID 2g/L
Oxyethyl group amino dodecane 3g/L
Virahol 8%
DMF 7％
P65 0.5g/L
All the other pure water
Wherein, P65 is a non-ionic type block macromolecular tensio-active agent, the component of ethylene oxide (EO) and propylene oxide (PO) is-(EO) 20-(PO) 30-(EO) 20-(PO) 30-.
Use the silver protecting agent of the embodiment of the invention 7, under following processing condition:
Join the groove ratio Treatment temp Treatment time Processing mode Post-treatment condition
100ml/L, all the other are water 50℃ 50 seconds Soak or spray Hot water cleans, again ultrasonic wave water cleaning, drying
Handle the silver layer protection effect that 1000 wiring board tests record
Deposit a week in the air Deposited in the air three months Deposited in the air six months 10％FeCl 3The solution destructive test
The nondiscoloration of silver face The nondiscoloration of silver face The nondiscoloration of silver face Silver-colored face nondiscoloration in 30 seconds
Solderability test:, print soldering paste (tin/copper/silver alloys) then respectively and cross reflow ovens and manual immersed solder test (265 ℃, tin/copper/silver alloys) through three to six reflow ovens (265 ℃ of top temperature, top 65 seconds time of temperature) baking
Figure A20071007289400101
Embodiment 8: the present invention is used for the protective material of silver layer surface, and its component and content are:
Benzene TETRADECONIC ACID 2g/L
Stearylamide 3g/L
Virahol 8%
DMF 7％
OP10 0.5g/L
All the other pure water
Use the silver protecting agent of the embodiment of the invention 8, under following processing condition:
Join the groove ratio Treatment temp Treatment time Processing mode Post-treatment condition
No. 1 100ml/L, all the other are water 50℃ 50 seconds Soak or spray Hot water cleans, again ultrasonic wave water cleaning, drying
Handle the silver layer protection effect that 1000 wiring board tests record
Deposit a week in the air Deposited in the air three months Deposited in the air six months 10％FeCl 3The solution destructive test
The silver face does not have the corrosion nondiscoloration The silver face does not have the corrosion nondiscoloration The silver face does not have the corrosion nondiscoloration Silver-colored face does not have the corrosion nondiscoloration in 30 seconds
Solderability test:, print soldering paste (tin/copper/silver alloys) then respectively and cross reflow ovens and manual immersed solder test (265 ℃, tin/copper/silver alloys) through three to six reflow ovens (265 ℃ of top temperature, top 65 seconds time of temperature) baking
Figure A20071007289400111

Claims (7)

1. anticorrosion preservative that is used for silver layer surface, it is characterized in that: the component of described anticorrosion preservative and content are:
Structure is R 1-(CH 2) n-R 2Filmogen 0.1g～10g/L
Solvent 1%～20% (V/V)
Tensio-active agent 0.1g～5g/L
Water surplus
Described structure is R 1-(CH 2) n-R 2Filmogen R 1Be phenyl, benzyl, alkene alkane, alkynes alkane, hydroxyl, carboxyl, alkoxyl group or alkyl, n=8～20, R 2For-COOH ,-NH 2,-SH ,-COONH 2,-S-S-R or-CN, described anticorrosion preservative comprises one or more described filmogen;
Described solvent is alcoholic solvent, contain the solvent of Ester and heterocycle material, water-soluble ethers kind solvent or polar solvent;
Described tensio-active agent is nonionogenic tenside or cats product.
2. the anticorrosion preservative that is used for silver layer surface according to claim 1 is characterized in that: described alcoholic solvent is that ethanol, butanols, Virahol, molecular weight are that 200～1000 polyoxyethylene glycol and/or molecular weight are 200～1800 polypropylene glycol.
3. the anticorrosion preservative that is used for silver layer surface according to claim 1 is characterized in that: described polar solvent is dimethyl formamide and/or dimethyl sulfoxide (DMSO).
4. the anticorrosion preservative that is used for silver layer surface according to claim 1 is characterized in that: described nonionogenic tenside is the segmented copolymer of alkyl alcohol polyethenoxy ether class or ethylene oxide and propylene oxide.
5. the anticorrosion preservative that is used for silver layer surface according to claim 1 is characterized in that: described cats product is a dodecyl benzyl dimethyl ammonium chloride.
6. the anticorrosion preservative that is used for silver layer surface according to claim 1 is characterized in that: also comprise co-solvent, content is 1%～10% (V/V).
7. the anticorrosion preservative that is used for silver layer surface according to claim 6 is characterized in that: described co-solvent is ethylene glycol, glycerol and/or glycol ether.
CNA2007100728945A 2007-01-19 2007-01-19 Anticorrosion preservative used for silver layer surface Pending CN101225259A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101974757A (en) * 2010-11-04 2011-02-16 西北工业大学 Water-soluble nickel protective agent as well as preparation method and use method thereof
CN102162095A (en) * 2011-03-01 2011-08-24 济南德锡科技有限公司 Anti-discoloring protective agent for silver plating and preparation method as well as application method thereof
CN104043571A (en) * 2014-07-09 2014-09-17 苏州东吴黄金文化发展有限公司 Coating process for preventing silver from darkening and denigrating
CN104419921A (en) * 2013-08-26 2015-03-18 比亚迪股份有限公司 Water soluble silver protective agent, preparation method thereof, chemical silvering method and surface silver plated workpiece
CN108070863A (en) * 2017-12-13 2018-05-25 扬州大学 A kind of surface protectant for silvering
CN108998796A (en) * 2018-08-20 2018-12-14 深圳市指尖坊黄金珠宝首饰有限公司 A kind of jewellery surface treating agent
CN109266076A (en) * 2018-08-27 2019-01-25 深圳市星扬高新科技有限公司 Silver surface protective agent and its application method

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101974757A (en) * 2010-11-04 2011-02-16 西北工业大学 Water-soluble nickel protective agent as well as preparation method and use method thereof
CN102162095A (en) * 2011-03-01 2011-08-24 济南德锡科技有限公司 Anti-discoloring protective agent for silver plating and preparation method as well as application method thereof
CN102162095B (en) * 2011-03-01 2012-08-08 济南德锡科技有限公司 Anti-discoloring protective agent for silver plating and preparation method as well as application method thereof
CN104419921A (en) * 2013-08-26 2015-03-18 比亚迪股份有限公司 Water soluble silver protective agent, preparation method thereof, chemical silvering method and surface silver plated workpiece
CN104419921B (en) * 2013-08-26 2017-07-21 比亚迪股份有限公司 A kind of water-soluble silver protecting agent and preparation method thereof, chemical silver plating method and electroplate workpiece
CN104043571A (en) * 2014-07-09 2014-09-17 苏州东吴黄金文化发展有限公司 Coating process for preventing silver from darkening and denigrating
CN104043571B (en) * 2014-07-09 2016-08-24 苏州东吴黄金文化发展有限公司 The coated technique of silver anti-darkening blackening
CN108070863A (en) * 2017-12-13 2018-05-25 扬州大学 A kind of surface protectant for silvering
CN108998796A (en) * 2018-08-20 2018-12-14 深圳市指尖坊黄金珠宝首饰有限公司 A kind of jewellery surface treating agent
CN109266076A (en) * 2018-08-27 2019-01-25 深圳市星扬高新科技有限公司 Silver surface protective agent and its application method

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Open date: 20080723