CN105002488B - A kind of metal coating surface protection method for sealing of wiring board and weld assembly - Google Patents
A kind of metal coating surface protection method for sealing of wiring board and weld assembly Download PDFInfo
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- CN105002488B CN105002488B CN201510400704.2A CN201510400704A CN105002488B CN 105002488 B CN105002488 B CN 105002488B CN 201510400704 A CN201510400704 A CN 201510400704A CN 105002488 B CN105002488 B CN 105002488B
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Abstract
The invention provides a kind of metal coating surface of wiring board and weld assembly protection method for sealing and a kind for the treatment of fluid for metal coating surface protection sealing of hole.The treatment fluid includes pretreatment fluid and aftertreatment fluid；According to mass percent meter, the pretreatment fluid includes C2‑C11Terminal hydroxy group alkyl hydrosulfide 0.02 2%, nonionic surfactant 0.01 5% and deionized water surplus；The aftertreatment fluid is silylating reagent.It is described protection method for sealing be：Test specimen with the coat of metal is immersed into pretreatment fluid to be pre-processed；Pretreated test specimen is cleaned with deionized water, dried；Dried test specimen is immersed in silylating reagent and post-processed.After treatment fluid sealing pores of the present invention, the decay resistance of the coat of metal significantly increases, and metal coating surface forms the organic film of compact strong-hydrophobicity, has good salt spray resistance, and do not influence the welding performance of the coat of metal.
Description
Technical field
The invention belongs to technical field of metal surface protection, and in particular to a kind of coat of metal of wiring board and weld assembly
Surfacecti proteon method for sealing and a kind for the treatment of fluid for metal coating surface protection sealing of hole.
Background technology
The copper metal face of wiring board and weld assembly, is easily corroded and is aoxidized in the environment.At present, copper metal is often adopted
Increase its corrosion resistance with the technique of plating inert metal.In general, it is usually used in the manufacture of assist side and weld assembly
Plating inert metal technique have it is following several：Nickel plating/gold-plated, nickel plating/plating palladium/gold-plated, nickel plating/silver-plated, nickel plating/plating palladium/silver-plated
Deng.
Gold/silver is inert metal, stable chemical performance, is highly resistant to harmful substance (such as H in air atmosphere2S、SO2、
CO2、NO2、CO2) erosion, (such as salt fog, mist of oil, mould, the air of humidity and hot conditions) can also protect in adverse circumstances
Deposit, be not easy corrosive chameleon；Gold/silver-colored resistivity is low simultaneously, easy welding, has good attachment with matrix materials such as copper, nickel, palladiums
Property.Therefore, gold/silver is widely used as the functional coating of wiring board and weld assembly.The coating of gold/silver must be continuously without micro-
Hole, surface is not oxidized or corrodes, and could effectively protect base metal.But in actual production, the defects of parent metal, bag
Include the set-up procedure of matrix and the roughness of parent metal, and the improper activity during plating process can trigger coating
Crystal defect, it is mainly shown as deformity crystallization and coating micropore.Metallic crystal at these crystal defects is in metastable state, easily
As the starting point of extraneous corrosion coating；Nanopores are easier to remain the impurity such as plating or the liquid medicine of leaching or auxiliary agent, tight so as to cause
The electrochemical corrosion of weight.Therefore, the coating of gold/silver is difficult to show as metal consistent high corrosion-resistant in itself, involved production
Product also are difficult to test by increasingly harsh reliability standard.Conventional solution method is to increase the thickness of inert metal layer, i.e.,
Using thick gold/silver process., can be blocking microporous because interlaced between metal level crystallization nucleus with the increase of thickness, make hole
Rate reduces, so as to reduce coat of metal oxide etch.But gold/silver is expensive, in addition in recent years international gold/silver-colored price it is continuous on
Rise, seriously exacerbate the production cost pressure of electronic component enterprise.In addition, thick gold/silver process can not fundamentally solve by
In coating oxidation caused by crystal defect (particularly fault location residue).Therefore, exploitation is a kind of can both make wiring board and weldering
Connected components keep solderability and reliability for a long time, and new technology or the product that can save gold/silvering dosage again are very urgent.
Conventional metal protection technique includes turn blue processing, coating treatment, phosphorating treatment, sealing pores.(1) turn blue processing
It is in air, vapor or containing NaOH, NaNO by the steel through over cleaning3Deng being heated to 140 DEG C or so in Oxidant, make
Steel surface generates one layer of fine and close blueness or black oxide film, and to improve the corrosion resistance of steel and outward appearance, this technique is referred to as turning blue
Processing.Oxide-film has Fe3O4Composition, thickness be 0.6~0.8 μm, compact structure, uniformly, be firmly combined with, can prevent with metal surface
Atmospheric corrosion.But wiring board and weld assembly need to carry out welding processing, oxide-film is solder base material in welding processing
Maximum resistance, it is clear that processing of turning blue is not suitable for the protection of wiring board or weld assembly.(2) coating treatment is that use will be supported
The polymeric (i.e. protective coating) for driving extraneous chemical attack is coated in metal surface, and metal is prevented by coating
Shield.But protective coating can equally influence the welding processing of wiring board and solder flux component, it is clear that coating treatment does not apply to yet.
(3) phosphorating treatment, the phosphorating treatment into row metal is first had to, i.e. workpiece is immersed in phosphate solution and heated, obtains its surface
Obtain one layer of densification, grey black phosphate film not soluble in water.Phosphate film (5-15 μm of thickness) and metallic matrix adhesion
It is very strong, it is not easy to peel off, it (removes H to air, lubricating oil, gaseous fuel and most of gas2S) there is good resistance to corrosion.
But phosphorating treatment produces and contains phosphorus waste liquid, causes environmental pollution；And phosphate film is equally solder in welding processing
The obstruction of base material so, phosphorating treatment is not suitable for the protection of wiring board or weld assembly.(4) sealing pores often use dichromic acid
Potassium is passivated to metal surface, is allowed to close the pin hole of the coat of metal, is prevented air oxidation.This is a kind of having for traditional row
The technique of effect, still, this sealing of hole process can produce chrome waste liquid, cause environmental pollution, and due to its toxicity problem, by
Prohibit the use of in most of industrial product.
The content of the invention
It is unfavorable for wiring board for anti-corrosion of metal processing technology in the prior art or the follow-up welding processing of weld assembly uses
The problem of with environmental pollution is easily caused, present invention proposition is a kind of to be used without influence, environmentally friendly circuit follow-up welding processing
The metal coating surface of plate and weld assembly protects the treatment fluid and application method of sealing of hole.
The first aspect of the invention is to provide a kind for the treatment of fluid for metal coating surface protection sealing of hole, and its feature exists
In the treatment fluid includes pretreatment fluid and aftertreatment fluid；According to mass percent meter, the pretreatment fluid includes C2-C11's
Terminal hydroxy group alkyl hydrosulfide 0.02-2%, nonionic surfactant 0.01-5% and deionized water surplus；The aftertreatment fluid is
Silylating reagent.
Further, the metal is gold or silver.It should be appreciated that the treatment fluid is readily applicable to other metals
Coating, such as copper, iron, zinc, platinum, nickel.
Further, the cloud point of the nonionic surfactant is >=50 DEG C.
Further, the cloud point of the nonionic surfactant is 50-80 DEG C.
Further, the HLB value of the nonionic surfactant is 12-14.
Nonionic surfactant can be polyethylene, be oxirane and compound addition containing active hydrogen and
Obtain, including APES (or ester), high-carbon fatty alcohol polyoxyethylene ether (or ester), the oxirane of polypropylene glycol add
Into thing (ester) etc..Nonionic surfactant can be polyol type, be ethylene glycol, glycerine pentaerythrite, anhydrous sorbitol and
The ester that the organic matter containing multiple hydroxyls such as sucrose is formed with higher fatty acids, including sorbitan ester, alkylolamides type
Deng.
Further, described silylating reagent is N, the double trimethyl silicon substrate trifluoroacetamides of O-, the double trimethyl silicanes of N, O-
Yl acetamide, N- methyl-N- (tert-butyl dimethylsilyl) trifluoroacetamide, N- methyl-N- (trimethylsilyl) trifluoro second
One or more in acid amides.
The second aspect of the invention is to provide a kind of metal coating surface protection method for sealing (first side i.e. of the invention
The application method for the treatment of fluid described in face), with the treatment fluid described in one side of the invention, prepare as steps described below and
Into：
Step 1, the test specimen with the coat of metal is immersed into pretreatment fluid to be pre-processed；
Step 2, pretreated test specimen is cleaned with deionized water, dried；
Step 3, dried test specimen is immersed in silylating reagent and post-processed.
Further, in step 1, the temperature of pretreatment fluid is 30-70 DEG C, pretreatment time 1-10min.
Further, in step 2, deionized water cleaning temperature is 30-50 DEG C, scavenging period 10s-60s.
Further, in step 3, silylating reagent post-processing temperature is 30-70 DEG C, finishing time 1-10min.
The present invention uses a kind of terminal hydroxy group alkyl hydrosulfide, Chinese synonym end sulfhydryl alkyl alcohol, molecular formula HO- (R)n-SH
(n=2-11) terminal hydroxy group alkyl hydrosulfide and nonionic surfactant, are configured to the aqueous solution, to wiring board and weld assembly
Metal surface coating is handled.Sulfydryl (- SH) in mercaptan is to the meta-stable metal crystal at crystal defect in the coat of metal
Self assembly is carried out, the terminal hydroxy group alkyl hydrosulfide after self assembly completely cuts off meta-stable metal crystal and extraneous corrosiveness, plays slow
The effect of erosion；Meanwhile the nonionic surfactant in pretreatment fluid, plating liquid medicine or auxiliary agent to nanopores residual etc. is miscellaneous
Matter plays the effects such as emulsification, scattered, hydrotropy, impurity is removed by effective cleaning, prevents electrochemical corrosion；In addition, pass through
The hydroxyl of silylating reagent and terminal hydroxy group alkyl hydrosulfide is reacted, and the silicon of strong-hydrophobicity is formed in the hole of gold/silvering
Alkanethiol alkyl film, further enhance the anticorrosion effect of sealing of hole.This silanethiol alkyl film, can be in the work of welding temperature
Decompose and destroy under, do not influence the use of the follow-up welding processing of wiring board and weld assembly.The sealing pores liquid, makes
With the unconfined environmentally friendly raw material of legislations of environmental protection, the activity component concentration in the terminal hydroxy group alkyl hydrosulfide aqueous solution used is low, raw
Waste liquid caused by production is handled through simple filtration can reach the requirement directly discharged.
The coat of metal object that the present invention protects is mainly：There is actual use to the surface metal of wiring board and weld assembly
Inert metal (i.e. gold/silver) coating of value.Shown according to the mechanism of action of the present invention and existing Research Literature：The present invention
Treatment fluid is readily applicable to other coats of metal, such as copper, iron, zinc, platinum, nickel.
Embodiment
It is unfavorable for wiring board for anti-corrosion of metal processing technology in the prior art or the follow-up welding processing of weld assembly uses
The problem of with environmental pollution is easily caused, present invention proposition is a kind of to be used without influence, environmentally friendly circuit follow-up welding processing
The metal coating surface of plate and weld assembly protects the treatment fluid and method of sealing of hole.The treatment fluid includes pretreatment fluid with after
Treatment fluid；According to mass percent meter, the pretreatment fluid includes C2-C11Terminal hydroxy group alkyl hydrosulfide 0.02-2%, nonionic
Surfactant 0.01-5% and deionized water surplus；The aftertreatment fluid is silylating reagent.In use, will be with the coat of metal
Test specimen immerse pretreatment fluid pre-processed；Pretreated test specimen is cleaned with deionized water, dried；By dried examination
Part, which is immersed in silylating reagent, to be post-processed.
Chemisorbed can occur between metal, metal oxide for the sulfydryl of alkyl hydrosulfide, and (Me refers to gold to formation-SMe
Category) and steady ordered self-composed monomolecular film., can only but alkyl hydrosulfide forms monomolecular film in metal surface
Play a part of inhibition, long-term corrosion resistance is not strong, is easily destroyed by such environmental effects.The present invention uses terminal hydroxy group alkane
Base mercaptan, silylating reagent processing is added in subsequent treatment, is effectively improved the corrosion resistance of alkyl hydrosulfide molecular film.
The present invention uses silylating reagent, and silylation is incorporated into terminal hydroxy group alkyl hydrosulfide, substitutes the activity of terminal hydroxy group
Hydrogen, reactive hydrogen reduce the polarity of whole compound after being substituted by silylation, improve hydrophobicity and stability, resistance to so as to improve
Corrosive nature.Silylating reagent is N in the present invention, the double trimethyl silicon substrate trifluoroacetamides of O-, the double trimethyl silicanes of N, O-
One kind in yl acetamide, N- methyl tertbutyl dimethyl silicon substrates trifluoroacetamide, N- methyl trimethoxy base silicon substrate trifluoroacetamides
It is or a variety of.
The present invention uses nonionic surfactant, compared to other ionics or amphoteric surfactant, so that it may dissolve
Property or dispersiveness, solubility, cost factor consider, be more applicable for sealing pores；In addition, in micropore remain plating liquid medicine or
Auxiliary agent, contain metal ion mostly, easy and ionic and amphoteric surfactant reaction, cause activating agent to fail, so
Nonionic surfactant is most suitable.Nonionic surfactant can be polyethylene, for oxirane and contain active hydrogen
Compound addition and obtain, including APES (or ester), high-carbon fatty alcohol polyoxyethylene ether (or ester), poly- the third two
Ethylene oxide adduct (ester) of alcohol etc..Nonionic surfactant can be polyol type, be ethylene glycol, glycerine Ji Wusi
The ester that the organic matter containing multiple hydroxyls such as alcohol, anhydrous sorbitol and sucrose is formed with higher fatty acids, including anhydrous sorbitol
Ester, alkylolamides type etc..Considered according to the factor such as solubility, dispersiveness, wetability, cost, preferably alkyl phenol polyoxy second
Alkene ether and AEO.
In addition, the addition concentration of nonionic surfactant, mass fraction 0.01-5% is substantially used in pretreatment fluid.It is non-
One or more additions can be used in ionic surface active agent.To make above-mentioned C2-C11 terminal hydroxy group alkyl hydrosulfide in aqueous
Can dispersed or dissolving, the preferred HLB value of nonionic surfactant be 12-14, cloud point >=50 DEG C (are more preferably 50-
80℃)." HLB " value is the ratio of the meaning of " hydrophile-lipophile balance ", hydrophilic radical and lipophilic group, using 0-20 numerical value come
Represent, from 0, more close relative's oiliness is higher, and from 20, more close relative is water-based higher.In addition, cloud point is the nonionic surfactant aqueous solution
In heating, the hydrogen in hydrophilic segment and water is combined and destroys hydrogen bond, and activating agent water solubility is drastically reduced, and solution, which is separated, to be become
Into the opaque temperature for starting that white casse is presented.Cloud point reflection nonionic surfactant hydrophily size, hydrophily are bigger
, cloud point is also higher.
In the context of the invention, unless otherwise specified, concentration is mass percentage concentration.
With reference to specific embodiment, the present invention is further illustrated, to more fully understand the present invention.
The preparation of test piece with the coat of metal：Using the conventional welding material copper metal of wiring board and weld assembly as examination
Part base material, the PROCESS FOR TREATMENT of nickel plating/gold-plated or nickel plating/silver-plated is carried out on copper surface, obtain the copper examination of surface band gold/silvering
Piece.
Embodiment 1
Using 0.02% hydroxyl ethyl mercaptan (carbon number=2), 0.01% OP-10 (OPEO,
C8H17C6H4O(CH2CH2O)nH (n=10), HLB：13.3-14 cloud point：68-78 DEG C) and the deionized water of surplus be configured to pre- place
Liquid is managed, pretreatment fluid is heated to 70 DEG C, the copper test piece with gold plate is immersed in pretreatment fluid and pre-processes 1min.
Pretreated test specimen, which is immersed in 30 DEG C of deionized water, cleans 10s, takes out, hot-air seasoning.
Test specimen after drying is immersed into N, the double trimethyl silicane yl acetamides of O-, 30 DEG C of processing 1min.
The test piece test result of the present embodiment sealing pores is shown in Table 1.
Embodiment 2
Using 2% hydroxyl butyl mercaptan (carbon number=4), 1% NP-9 (NPE, C9H19C6H4O
(CH2CH2O)nH (n=9), HLB：13.3-14 cloud point：68-78 DEG C) and the deionized water of surplus be configured to pretreatment fluid, will be pre-
Treatment fluid is heated to 30 DEG C, and the copper test piece of silvering is immersed in the terminal hydroxy group alkyl hydrosulfide aqueous solution and pre-processes 5min.
Pretreated test specimen, which is immersed in 40 DEG C of deionized water, cleans 60s, takes out, hot-air seasoning.
Test specimen after drying is entered into N- methyl-N- (tert-butyl dimethylsilyl) trifluoroacetamide, 70 DEG C of processing
10min。
The test piece test result of the present embodiment sealing pores is shown in Table 1.
Embodiment 3
Using 1% hydroxyl undecyl mercaptan (carbon number=11), 5% AEO-7 (AEO R-O-
(CH2CH2O)nH (R=C12-18, n=7), HLB：12.1 cloud point：>=50 DEG C) and the deionized water of surplus be configured to pretreatment fluid,
Pretreatment fluid is heated to 50 DEG C, the copper test piece with gold plate is immersed in the terminal hydroxy group alkyl hydrosulfide aqueous solution and pre-processes 3min.
Pretreated test specimen, which is immersed in 50 DEG C of deionized water, cleans 50s, takes out, hot-air seasoning.
Test specimen after drying is entered into N- methyl-N- (trimethylsilyl) trifluoroacetamide, 60 DEG C of processing 5min.
The test piece test result of the present embodiment sealing pores is shown in Table 1.
Embodiment 4
Pre- place is configured to using the deionized water of 0.1% hydroxyl hexyl mercaptans (carbon number=6), 0.5% NP-9 and surplus
Liquid is managed, pretreatment fluid is heated to 52 DEG C, the copper test piece with silvering is immersed in the terminal hydroxy group alkyl hydrosulfide aqueous solution and pre-processed
10min。
Pretreated test specimen, which is immersed in 40 DEG C of deionized water, cleans 30s, takes out, hot-air seasoning.
Test specimen after drying is entered into N, the double trimethyl silicon substrate trifluoroacetamides of O-, 30 DEG C of processing 10min.
The test piece test result of the present embodiment sealing pores is shown in Table 1.
Embodiment 5
Using 0.2% hydroxypropyl mercaptan (carbon number=3), 2% OP-9 (OPEO, C8H17C6H4O
(CH2CH2O)nH (n=9), HLB：12.5-12.7 cloud point：60-65 DEG C) and the deionized water of surplus be configured to pretreatment fluid, will
Pretreatment fluid is heated to 60 DEG C, and the copper test piece with gold plate is immersed in the terminal hydroxy group alkyl hydrosulfide aqueous solution and pre-processes 6min.
Pretreated test specimen, which is immersed in 40 DEG C of deionized water, cleans 50s, takes out, hot-air seasoning.
Test specimen after drying is entered into N, the double trimethyl silicane yl acetamides of O-, 50 DEG C of processing 3min.
The test piece test result of the present embodiment sealing pores is shown in Table 1.
Embodiment 6
It is configured to pre-process using the deionized water of 0.5% hydroxypropyl mercaptan (carbon number=3), 4% OP-9 and surplus
Liquid, pretreatment fluid is heated to 60 DEG C, the copper test piece with silvering is immersed in the terminal hydroxy group alkyl hydrosulfide aqueous solution and pre-processed
6min。
Pretreated test specimen, which is immersed in 40 DEG C of deionized water, cleans 40s, takes out, hot-air seasoning.
Test specimen after drying is entered into N, the double trimethyl silicon substrate trifluoroacetamides of O-, 60 DEG C of processing 2min.
The test piece test result of the present embodiment sealing pores is shown in Table 1.
Embodiment 7
Prepared using the deionized water of 1% hydroxyl hexyl mercaptans (carbon number=6), 1% NP-9,1% AEO-7 and surplus
Into pretreatment fluid, pretreatment fluid is heated to 60 DEG C, the copper test piece with gold plate is immersed in the terminal hydroxy group alkyl hydrosulfide aqueous solution
Pre-process 5min.
Pretreated test specimen, which is immersed in 45 DEG C of deionized water, cleans 60, takes out, hot-air seasoning.
Test specimen after drying is entered into N, the double trimethyl silicon substrate trifluoroacetamides of O-, the double trimethyl silicane yl acetamides of N, O-,
N- methyl-N- (tert-butyl dimethylsilyl) trifluoroacetamide, four kinds of N- methyl-N- (trimethylsilyl) trifluoroacetamide are pressed
The mixed silanes reagent that the ratio that mass ratio is 1/1/1/1 is prepared, 60 DEG C of processing 5min.
The test piece test result of the present embodiment sealing pores is shown in Table 1.
The test piece that embodiment 1 to 6 is obtained and the test piece without sealing pores carry out following corresponding test.
(1) salt spray test, with reference to chinese national standard " GB/T 10125-1997 artificial atmosphere corrosion tests salt spray test "
Tested, testing time selection 24h, 48h, 72h.The evaluation criterion of salt fog performance corrosion see the table below：
| Rank | Corrosion condition describes |
| 0 grade | Without any corrosion |
| 1 grade | The corrosion location area of test piece is less than 10% |
| 2 grades | The corrosion location area of test piece is more than 10%, less than 30% |
| 3 grades | The corrosion location area of test piece is more than 30% |
(2) hydrophobicity is tested, and with reference to chinese national standard, " GB/T 24368-2009 glass surfaces hydrophobic contaminants detect
Contact-angle measurement method " is tested.
(3) solderability is tested, with reference to chinese national standard " GB/T 9491-2002 solderings with liquid flux (abietyl) "
In the 5.8.1 rates of spread tested.Test condition is：To meet the superfine solid rosin of GB/T 8145 be dissolved in absolute ethyl alcohol or
In isopropanol, the mass percent for making rosin is 25%, obtains testing scaling powder used；Solder use the trade mark for
HI.SnPb39 tin-leads；235 DEG C of test temperature.
The embodiment 1 to 6 of table 1 and the test result without sealing pores
From upper table data：By the copper test piece of band gold/silvering of sealing pores of the present invention, no sealing pores are contrasted
Test piece, salt spray corrosion resistance and water resistance be all significantly improved, wherein, embodiment 2,3,6 and 7, in salt spray test 48h
Afterwards, the corrosion-free phenomenon in surface, illustrate gold/silvering under this four hole-sealing technology processing, there is good antiseptic property.This
It is that gold/silvering surface occurs self assembly by terminal hydroxy group alkyl hydrosulfide and metal and made because after sealing pores of the present invention
With chemisorbed terminal hydroxy groups alkyl hydrosulfide molecule.The hydroxyl of terminal hydroxy group alkyl hydrosulfide is after silanization treatment, in gold/silver plating
Layer surface forms organic monomolecular film, plays good hydrophobicity (isolation steam) and decay resistance.In addition, from the rate of spread
Data find out, sealing pores of the present invention on the solderability of gold/silvering substantially without influence, suitable for wiring board and weld assembly
Protecting metallic surface processing.
The specific embodiment of the present invention is described in detail above, but it is intended only as example, it is of the invention and unlimited
It is formed on particular embodiments described above.To those skilled in the art, it is any to the equivalent modifications that carry out of the present invention and
Substitute also all among scope of the invention.Therefore, the impartial conversion made without departing from the spirit and scope of the invention and
Modification, all should be contained within the scope of the invention.
Claims (6)
1. a kind for the treatment of fluid for metal coating surface protection sealing of hole, it is characterised in that the treatment fluid includes pretreatment fluid
And aftertreatment fluid；According to mass percent meter, the pretreatment fluid includes C2-C11Terminal hydroxy group alkyl hydrosulfide 0.02-2%, non-
Ionic surface active agent 0.01-5% and deionized water surplus；The aftertreatment fluid is silylating reagent.
2. treatment fluid according to claim 1, it is characterised in that the metal is gold or silver.
3. treatment fluid according to claim 1, it is characterised in that the cloud point of the nonionic surfactant is >=50
DEG C, the HLB value of the nonionic surfactant is 12-14.
4. treatment fluid according to claim 3, it is characterised in that the cloud point of the nonionic surfactant is 50-80
℃。
5. treatment fluid according to claim 1, it is characterised in that described silylating reagent is N, the double trimethyl silicon substrates of O-
Trifluoroacetamide, N, the double trimethyl silicane yl acetamides of O-, N- methyl-N- (tert-butyl dimethylsilyl) trifluoroacetamide, N- first
One or more in base-N- (trimethylsilyl) trifluoroacetamide.
6. a kind of metal coating surface protects method for sealing, it is characterised in that using described in any one in claim 1-5
Treatment fluid, carry out as steps described below：
Step 1, the test specimen with the coat of metal is immersed into pretreatment fluid to be pre-processed；
Step 2, pretreated test specimen is cleaned with deionized water, dried；
Step 3, dried test specimen is immersed in silylating reagent and post-processed；
In step 1, the temperature of pretreatment fluid is 30-70 DEG C, pretreatment time 1-10min；In step 2, deionized water cleaning
Temperature is 30-50 DEG C, scavenging period 10s-60s；In step 3, silylating reagent post-processing temperature is 30-70 DEG C, post processing
Time is 1-10min.
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| CN201510400704.2A CN105002488B (en) | 2015-04-10 | 2015-07-08 | A kind of metal coating surface protection method for sealing of wiring board and weld assembly |
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| CN109690365B (en) * | 2015-10-19 | 2022-08-23 | 美题隆公司 | Corrosion resistant optical device |
| CN106337196B (en) * | 2016-07-31 | 2018-08-10 | 深圳市贝加电子材料有限公司 | Microscopic void sealer for the processing of printed wiring board precious metal surface |
| CN110055523B (en) * | 2019-04-19 | 2021-05-07 | 佛山市因信贵金属材料有限公司 | Water-based silver protective agent and preparation method thereof |
| CN110416782A (en) * | 2019-08-27 | 2019-11-05 | 问问智能信息科技有限公司 | A kind of charging contact composite structure and preparation method thereof |
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| CN102747350A (en) * | 2012-07-18 | 2012-10-24 | 深圳市成功科技有限公司 | Gold/silver plating layer surface protective agent |
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| JP2013072096A (en) * | 2011-09-27 | 2013-04-22 | Hitachi Ltd | Organic-inorganic composite and method for manufacturing the same |
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| CN102747350A (en) * | 2012-07-18 | 2012-10-24 | 深圳市成功科技有限公司 | Gold/silver plating layer surface protective agent |
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