CN110468394A - A kind of silver-based wiring board of chemical nickel plating porpezite and preparation method thereof - Google Patents
A kind of silver-based wiring board of chemical nickel plating porpezite and preparation method thereof Download PDFInfo
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- CN110468394A CN110468394A CN201910709955.7A CN201910709955A CN110468394A CN 110468394 A CN110468394 A CN 110468394A CN 201910709955 A CN201910709955 A CN 201910709955A CN 110468394 A CN110468394 A CN 110468394A
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
- C23C18/1651—Two or more layers only obtained by electroless plating
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1837—Multistep pretreatment
- C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
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- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Electroplating Methods And Accessories (AREA)
- Chemically Coating (AREA)
- Manufacturing Of Printed Wiring (AREA)
Abstract
The invention discloses silver-based wiring board of a kind of chemical nickel plating porpezite and preparation method thereof, the silver-based wiring board includes silver-based substrate, and the surface of the silver-based substrate is successively plated with nickel layer, palladium layers, layer gold from the inside to the outside.The preparation method, the following steps are included: by cleaned treated silver-based substrate successively carries out microetch, pickling, pre- pickling, palladium activation, rear pickling pre-treatment, the silver-based substrate through pre-treatment is subjected to chemical nickel plating, chemical palladium-plating, chemical gilding successively up to the silver-based wiring board of the coating containing NiPdAu again, for traditional copper-based chemical nickel plating porpezite, the thickness of NiPdAu chemical deposit can be greatly lowered, to save the use content of metal, while avoiding the problem that polluting the environment.Furthermore using silver-based as substrate, entire product is conductive, thermal conductivity is stronger, sensitivity is higher, longer life expectancy, and overall performance is more excellent.
Description
Technical field
The present invention relates to silver-based wiring boards of a kind of chemical nickel plating porpezite and preparation method thereof, belong to process of surface treatment skill
Art field.
Background technique
With the high speed development of electronics industry, the demand of wiring board is growing day by day.But electronic product of today by
Gradually develop to directions such as multi-functional, high-performance, portable reliable low costs, the needs of in order to meet market and technology, not only wants
Ask electronic-packaging processes that must move towards system encapsulation or the highdensity encapsulation of IC package, it is a variety of that this just needs one kind to be able to satisfy
The coating of packaging technology, therefore thus " omnipotent " good reputation of chemical nickel plating porpezite process of surface treatment generates.
Chemical nickel plating porpezite main technique is chemical nickel plating, chemical palladium-plating and chemistry leaching are golden, wherein each step process
Processing all generates strong influence to the performance of product, and the superiority and inferiority of coating decides the quality of the performance of entire product.
Currently used chemical plating substrate be it is copper-based, but microetch it is processed after copper-based pollution and oxygen vulnerable to environment
Change.Simultaneously use copper-based substrate, generally require thicker nickel layer and palladium layers, with prevent copper-based base oxidation and stop copper ion to
The diffusion of layer gold, the migration to circuit board surface, causes the problem of product solderability difference.Furthermore it is used in combination with performance and life
Cost etc. being produced because usually considering, many persons select nickel chemical plating technology and replace chemical gilding technique, but nickel chemical plating technology
It is poor to beat gold thread binding ability, it is difficult to form competitive advantage and expanded.But simple chemical gilding technique, then cause noble metal
A large amount of uses, both cost of idleness, and easily polluting the environment.
And silver-based is relative to copper-based, conduction, thermal conductivity, sensitivity will it is excellent very much, be expected to produce to lead
The strong high-quality wiring board of electricity, good heat conductivity, high sensitivity, erosion resistant and inoxidizability, however do not have also in currently available technology
Have and uses using silver-based as the process of the chemical nickel plating porpezite of substrate.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of good heat conductivity, high sensitivity, erosion resistant and inoxidizability
Strong silver-based wiring board of chemical nickel plating porpezite and preparation method thereof
To achieve the goals above, the invention provides the following technical scheme:
A kind of silver-based wiring board of chemical nickel plating porpezite of the present invention, the silver-based wiring board include silver-based substrate, the silver
The surface of base substrate is successively plated with nickel layer, palladium layers, layer gold from the inside to the outside.
A kind of preparation method of the silver-based wiring board of chemical nickel plating porpezite of the present invention, includes the following steps: cleaned place
Silver-based substrate after reason successively carries out microetch, pickling, pre- pickling, palladium activation, rear pickling pre-treatment, then by the silver-based through pre-treatment
Substrate carries out chemical nickel plating, chemical palladium-plating, chemical gilding successively up to the silver-based wiring board of the coating containing NiPdAu.
Preferred scheme, the cleaning treatment process are as follows: silver-based substrate is first cleaned into 10~15min with ultrapure water, then
Oil removal treatment is carried out again, except oxide process；The oil removal treatment uses the dodecyl sodium sulfate of mass fraction 3%~5%
With the mixed solution of 20~30g/L sodium hydroxide, methane sulfonic acid, chloric acid, the high chlorine that 30mL/L is used except oxide process
The mixture of at least one of acid, nitric acid with 50~80g/L lauryl ammonium chloride.
The impurity such as the dust of ultrapure water cleaning silver-based substrate are used during cleaning treatment, and after cleaning, product is successively put
Enter oil removing, except in the detergent of oxide, sonic oscillation be added, completely remove the polluters such as fingerprint, greasy dirt of plate face source with
And oxide existing for silver-based surface, hot water wash and double water washing operations are then successively carried out again.When hot water wash, treatment temperature is
55~65 DEG C, the processing time is 1~3min, and double washings carry out for product to be placed in the lasting and uniform second level sink of water flow
2~3min is handled, the remaining acidic materials of plate face, i.e. acidic cleaning are washed away.
Preferred scheme, the microetch process be, cleaned treated silver-based substrate is placed in by oxide and microetch
In the mixed solution of acid, 2~3min is handled at 20~30 DEG C；The concentration of the oxide is 60~120g/L, microetch acid
Concentration is 15~40mL/L；Any one of the oxide in potassium permanganate, hydrogen peroxide, the microetch acid are selected from nitre
Acid, chloric acid, any one in methane sulfonic acid.
What the present invention initiated carries out chemical nickel plating porpezite by substrate of silver-based, inventors have found that smoothly in chemistry
The homogeneous coating with excellent electrical and thermal conductivity performance is obtained during plating, the pretreatment of early period is of crucial importance, if using existing
Hydrochloric acid system or sulfuric acid system in technology, due to the chloride ion contained in hydrochloric acid, the sulfate ion contained in sulfuric acid can
Precipitating occurs on silver-based surface or forms insoluble matter, not only will increase the difficulty of subsequent chemistry plating NiPdAu technique in this way, it is uneven
It is even, or even there is the problem of can not plating Shang Qu, and the performances such as its conductive and heat-conductive can be seriously affected, the present invention is through a large number of experiments
Every technique of pre-treatment is modified, is provided the foundation to form the strong NiPdAu coating of uniform associativity, such as in this hair
In bright microetch pretreatment process, using hydrogen peroxide as oxidant, with nitric acid, chloric acid, perchloric acid, in methane sulfonic acid at least
A kind of acidic environment of offer effect carries out microetch processing to plate face, make surface formed it is slight sting erosion layer, obtain fresh silver
Face provides better binding force for subsequent plating layer.
Inventors have found that microetch processing has larger impact to subsequent plating NiPdAu, it is necessary first to using above-mentioned specific
The combination of oxidant and acid, secondly the concentration of oxidant and acid is also required to effectively control.The concentration of oxidant is not enough or acid is dense
It spends low, it will the bad problem of the size uniformity degree of the depth deficiency and microetch aperture that cause microetch hole, this will be subsequentization
It learns nickel coating and increases difficulty, so that nickel coating uneven coating, binding force are poor.The excessive concentration or acid concentration of oxidant are excessively high,
By the depth that will cause microetch hole is too deep and the excessive problem in microetch aperture, this will destroy wiring board silver layer substrate, so that product
The excellent performance of silver layer substrate is reduced, and wastes reagent, increases the investment of cost, causes damages.
As a further preference, any one of the oxide and microetch acid in combining as follows: hydrogen peroxide
With chloric acid；Hydrogen peroxide and methane sulfonic acid, potassium permanganate and methane sulfonic acid.
In above-mentioned further preferred combination, after microetch processing, silver layer surface is smooth, smooth；Microetch uniform pore diameter
Preferably, surface roughness is small；Micro-corrosion liquid stable system, controllable-rate；Nickel plating after microetch, nickel layer binding force are strong.
Preferred scheme, the acid cleaning process are as follows: the silver-based substrate that will be handled through microetch, being placed in concentration is 80~120mL/
In the pickling solution of L, 1~3min is handled；The pickling solution is selected from nitric acid solution, solution chlorate, perchloric acid solution, methyl sulphur
At least one of acid solution.
The pre- pickling process of acid cleaning process, product is put into pickling solution and carries out pickling, removes preposition remaining micro-etching agent,
Then double water washing operations are carried out again, and the processing time is 2~3min, removes the remaining preposition medical fluid of plate face.
Preferred scheme, the pre- pickling process are as follows: by the silver-based substrate through pickling processes, being placed in concentration is 6~12mL/
In the pre- pickling solutions of L, 1~3min is handled；The pre- pickling solutions are selected from nitric acid solution, solution chlorate, perchloric acid solution, first
At least one of base sulfonic acid solutions.
During pre- pickling, the silver-based substrate through pickling processes is put into pre- pickling solutions, the acid of silver layer activation is provided
Property environment, make the plate face of wiring board in anaerobic state, and ensure that subsequent activating solution is not brought into excessive water and is diluted.
Preferred scheme, the palladium activation process are as follows: the silver-based substrate that will be handled through pre- pickling is placed in palladium activating solution,
In 20~30 DEG C, 2~3min is handled, the palladium activating solution is made of acid with the palladium salt of corresponding acid ion, and the acid is selected from nitre
Any one in acid, chloric acid, perchloric acid or methyl acid；The concentration of the acid is 60~100mL/L；The palladium of corresponding acid ion
The concentration of salt is 60~120mL/L.
After palladium activation, one layer of activation palladium is deposited in silver layer surface, provides catalytic action for subsequent nickel plating.After palladium activation, need
Wiring board is subjected to double water washing operations, the processing time is 2~3min, removes the remaining preposition medical fluid of plate face.
Preferred scheme, it is described after pickling process are as follows: the silver-based substrate that will be activated through palladium, be placed in concentration be 15~
In the rear pickling solutions of 40mL/L, 1~3min is handled, the rear pickling solutions are molten selected from nitric acid solution, solution chlorate, perchloric acid
At least one of liquid, methanesulfonic acid solution.
Afterwards during pickling, the product after cleaning is put into rear pickling solutions, is removed remaining in wiring board plate face
Palladium activating compounds.Afterwards after pickling, wiring board need to be carried out to double water washing operations, the processing time is 2~3min, and it is residual to remove plate face
The preposition medical fluid stayed.
Preferred scheme, the nickel process are as follows: by the silver-based substrate that pickling is handled after, be placed in chemical nickel-plating liquid
Middle progress chemical nickel plating processing, the pH for controlling chemical nickel-plating liquid is 3.0~4.5, and temperature is 85~90 DEG C, chemical nickel plating processing
Time is 25~40min.
As a further preference, the chemical nickel-plating liquid includes following composition: 25~35g/L of nickel sulphonic acid, hypophosphorous acid
20~40g/L of sodium, 10~15g/L of sodium citrate, 15~25g/L of lactic acid, propionic acid 5-15g/L；35~50mg/L of Potassiumiodate, PPS
(propane sulfonic acid pyridinium salt) 5~10mg/L, DEP (N, N- diethyl propargylamine) 5~10mg/L.
Chemical Ni-plating layer is the direct contact layer with silver-colored base board, and inventor through a large number of experiments, preferably goes out with sulfonic acid
Nickel is nickel main salt, and sodium hypophosphite is reducing agent, and sodium citrate, lactic acid, propionic acid three serve as complexing agent, accelerator and solution buffering
Agent, Potassiumiodate are stabilizer, and PPS, DEP are surfactant, are carried out on silver-based substrate using formula provided by the present invention
Nickel plating, gained chemical Ni-plating layer are smooth；Porosity is low, and corrosion resistance of coating is extremely strong；Bath stability is fabulous；Plating speed is moderate；In conjunction with
Power is good；Brightness is good.
In formula for chemical plating nickel of the present invention, all medicaments are indispensable, and mutually collaboration could obtain optimal effect,
Such as propionic acid serves as the effect of accelerator in chemical nickel plating, while by synergistic effect, can make up caused by being added because of lactic acid
Plate face it is more coarse as a result, the leveling effect of plate face can be improved in the propionic acid appropriate that is added, obtain more smooth bright and clean plating
Layer.
The addition of any medicament simultaneously, component content is also critically important, is such as added excessively, greatly may cause plating solution not
Stablize or occur phenomena such as plating solution poisons.If such as adjustment propionic acid content is 30g/L or more, hence it is evident that visible plating solution plating speed adds
Fastly, the problems such as bath stability is deteriorated, and phosphorus content in deposited nickel layer can be made to increase, reduce high temperature resistant, erosion resistant of product etc.
Performance.
As a further preference, the chemical nickel-plating liquid includes following composition: nickel sulphonic acid 30g/L, sodium hypophosphite
30g/L, lactic acid 20g/L, propionic acid 10g/L, sodium citrate 12g/L, Potassiumiodate 45mg/L, PPS 8mg/L, DEP 8mg/L.
By chemical nickel plating, good, the fine and close metal nickel layer of one layer of binding force is formed on silver-based surface；Then double washings remove
Remaining plating nickel reagent.
Preferred scheme, the chemical palladium-plating process are as follows: the silver-based substrate that will be handled through chemical nickel plating is placed in chemical palladium-plating
Chemical palladium-plating processing is carried out in liquid, the pH for controlling chemical palladium plating solution is 4.5~6.5, and temperature is 48~52 DEG C, chemical palladium-plating processing
Time be 25~40min.
In the present invention, after carrying out nickel plating, then when carrying out the plating of other coating, environment basic oneself and prior art copper
Environment after the wiring boards nickel plating such as base is identical, and the acid ion of other effects has no significant effect substrate silver layer, therefore existing skill
Conventional chemical palladium plating solution may be applicable to technical solution of the present invention in art.
As a further preference, the chemical palladium plating solution includes following composition: 1.2~1.5g/L of palladium nitrate, hypophosphorous acid
8~12g/L of sodium, 25~40g/L of ethylenediamine, triethanolamine 20g~30g/L, 15~25g/L of citric acid, 6~12g/ of ammonium citrate
L, 20~30mg/L of alkyl thiourea, 15~25mg/L of sodium thiosulfate.
Chemical palladium-plating is carried out by above-mentioned preferred chemical palladium plating solution, gained palladium coating is bright uniformly；Binding force is strong；It is anti-corrosion
Property is good；Bath stability is good, and MTO is greater than 6.
By chemical palladium-plating, one layer of metal palladium layers are formed on nickel layer surface；Then double washings remove remaining plating palladium reagent.
The processing time is 2~3min.
Preferred scheme, the chemical gilding process are as follows: the silver-based substrate that will be handled through chemical palladium-plating is placed in chemical gilding
Chemical gilding processing is carried out in liquid, the pH for controlling chemical gold plating liquid is 5.8~6.2, and temperature is 82~85 DEG C, chemical gilding processing
Time be 8~12min.
As a further preference, the chemical gold plating liquid includes following composition: 2.0~4.0g/L potassium auricyanide, 100
~120mL/L potassium hydroxide.
By chemical gilding, one layer of thin gold is formed on palladium layers surface, completes the chemical nickel plating porpezite on wiring board silver-based surface
Plating process.
Preferred scheme, the silver-based substrate that will be handled through chemical gilding, is first placed in normal-temperature water, is then placed in 55~65 again
DEG C water in, handle 1~3min to get the coating containing NiPdAu silver-based wiring board.
Product is immersed in the sink for filling clear water, the remaining gold-containing solution of plate face is sufficiently recycled, avoids the wave to gold salt
Take, and reduce the pollution to environment, subsequent hot water cleaning thoroughly removes the remaining preposition medical fluid of plate face, obtains and plate containing NiPdAu
The silver-based wiring board of layer.
Beneficial effect
The present invention initiates the progress chemical nickel plating palladium on silver-based substrate, and equal from pre-treating technology to nickel chemical plating technology
Form the technique for being most adapted to silver-based, chemical nickel plating porpezite of present invention on the basis of silver-based, compared to traditional copper-based chemical plating
For NiPdAu, the thickness of NiPdAu chemical deposit can be greatly lowered, to save the use content of metal, while avoiding pair
The problem of environment pollutes.Furthermore using silver-based as substrate, entire product is conductive, thermal conductivity is stronger, sensitivity is higher, the service life
Longer, overall performance is more excellent.
Specific embodiment
In order to keep being more clear for the purpose of the present invention, advantage and technical solution clear, next will make for the present invention
More detailed research.It is explained in conjunction with specific example.
Example is only preferred embodiment provided by the invention in detail below.
Embodiment 1
Cleaning: silver-based substrate is put into the super sink for filling ultrapure water, submerges silver-based substrate, is applied under room temperature light
Micro-vibration handles 10min, removes the impurity such as the dust of silver-based plate face.Product is put into the dodecyl sulphur of mass fraction 3% again
Sonic oscillation oil removal treatment is carried out in the mixed solution of sour sodium and 20g/L sodium hydroxide；Using 50g/L lauryl ammonium chloride with
30mL/L chloric acid mixture sonic oscillation is carried out except oxide process.
Microetch processing: by the silver-based substrate of above-mentioned cleaned processing, chloracid 30mL/L and hydrogen peroxide 100g/L are placed in
Mixed solution in carry out microetch processing, treatment temperature be 25 DEG C, time 2min, microetch processing after, silver layer surface is more smooth,
It is more smooth；Microetch aperture is more uniform, and surface roughness is smaller；Micro-etching speed is larger, and microetch system is more stable, controllable-rate.
Pickling: the silver-based substrate handled through microetch is placed in the nitric acid solution that concentration is 100mL/L, handles 2min.
Pre- pickling: by the nitric acid solution that concentration is 10mL/L of being placed in through pickling processes, 2min is handled.
Palladium activation, the silver-based substrate that will be handled through pre- pickling are placed in nitric acid containing 90mL/L and the palladium nitrate of 80mL/L
In palladium activating solution, in 25 DEG C, 2min is handled.
Pickling afterwards: the silver-based substrate that will be activated through palladium is placed in the nitric acid solution that concentration is 20mL/L, processing
2min。
Chemical nickel plating: by the silver-based substrate that pickling is handled after, progress chemical nickel plating processing in chemical nickel-plating liquid, control are placed in
The pH of chemical nickel-plating liquid processed is 3.0, and temperature is 85 DEG C, and the time of chemical nickel plating processing is 25min, and the group of chemical nickel-plating liquid becomes
Nickel sulphonic acid 30g/L, sodium hypophosphite 30g/L, lactic acid 20g/L, propionic acid 10g/L, sodium citrate 12g/L, Potassiumiodate 45mg/L, PPS
8mg/L,DEP 8mg/L.Chemical Ni-plating layer is smooth；Porosity is low, and detection resulting value is 0.11/cm2, corrosion resistance of coating pole
By force；Bath stability is fabulous；Plating speed is 34.5 μm/h；Binding force is good；Brightness is good.
Chemical palladium-plating: by the substrate containing nickel coating, it is placed in progress chemical palladium-plating processing in chemical palladium plating solution, controls chemical plating
The pH of palladium liquid is that 4.5 temperature are 48 DEG C, and the time of chemical palladium-plating processing is 25min, the formula of chemical palladium plating solution are as follows: palladium nitrate
1.2g/L, sodium hypophosphite 8g/L, ethylenediamine 25g/L, triethanolamine 20g/L, citric acid 15g/L, ammonium citrate 6g/L, alkyl sulfide
Urea 20mg/L, sodium thiosulfate 15mg/L.
Chemical gilding: by the substrate of nickeliferous palladium coating, progress chemical gilding processing, controlization in chemical gold plating liquid are placed in
It is 82 DEG C that the pH for learning gold plating liquid, which is 5.8 temperature, and the time of chemical gilding processing is 10min, the formula of chemical gold plating liquid are as follows: cyaniding
Golden potassium 3.0g/L, potassium hydroxide 100mL/L.
Product is put into the sink for filling clear water, sufficiently recycles the remaining gold-containing solution of plate face, then product is placed in temperature
Degree thoroughly removes the remaining medical fluid of plate face, obtains silver-based-NiPdAu route to carry out processing 1min in 55 DEG C of hot water.
Assessment of performance: 1 products obtained therefrom solderability of embodiment is stronger, and weldability is good；Good bonding strength uses heating pulling method
Measurement bond strength is 2892gf；Corrosion resistance is strong；With the copper-based pcb board ratio (thermal coefficient 16.5W/mK) of tradition, product is led
Hot coefficient is improved to 20.8W/mK, improves 26%, and thermal conductivity is high, and it is uniform to radiate.Can be perfectly suitable for it is heat-resisting to product,
The anti-corrosion equal higher field of performance requirements.
Embodiment 2
Cleaning: silver-based substrate is put into the super sink for filling ultrapure water, submerges silver-based substrate, is applied under room temperature light
Micro-vibration handles 10min, removes the impurity such as the dust of silver-based plate face.Product is put into the dodecyl sulphur of mass fraction 4% again
Sonic oscillation oil removal treatment is carried out in the mixed solution of sour sodium and 25g/L sodium hydroxide；Using 60g/L lauryl ammonium chloride with
30mL/L methane sulfonic acid mixture sonic oscillation is carried out except oxide process.
Microetch processing: by the silver-based substrate of above-mentioned cleaned processing, 30mL/L containing methane sulfonic acid and hydrogen peroxide are placed in
Microetch processing is carried out in the mixed solution of 100g/L, treatment temperature is 25 DEG C, time 2min, after microetch processing, silver layer surface
It is more smooth, it is more smooth；Microetch aperture is more uniform, and surface roughness is smaller；Micro-etching speed is larger, and microetch system is more stable, speed
Rate is controllable.
Pickling: the silver-based substrate handled through microetch is placed in the methanesulfonic acid solution that concentration is 100mL/L, processing
2min。
Pre- pickling: by the methanesulfonic acid solution that concentration is 10mL/L of being placed in through pickling processes, 2min is handled.
Palladium activation, the silver-based substrate that will be handled through pre- pickling are placed in methane sulfonic acid containing 90mL/L and the methyl of 80mL/L
In the palladium activating solution of sulfonic acid palladium, in 25 DEG C, 2min is handled.
Pickling afterwards: the silver-based substrate that will be activated through palladium is placed in the methanesulfonic acid solution that concentration is 20mL/L, processing
2min。
Chemical nickel plating: by the silver-based substrate that pickling is handled after, progress chemical nickel plating processing in chemical nickel-plating liquid, control are placed in
The pH of chemical nickel-plating liquid processed is that 4.0 temperature are 85 DEG C, and the time of chemical nickel plating processing is 30min, and the group of chemical nickel-plating liquid becomes
Nickel sulphonic acid 30g/L, sodium hypophosphite 30g/L, lactic acid 10g/L, propionic acid 5g/L, sodium citrate 5g/L, Potassiumiodate 45mg/L, PPS
8mg/L,DEP 8mg/L.Through detecting, chemical Ni-plating layer is more smooth；Porosity is lower, and detection resulting value is 2.2/cm2, coating
Corrosion resistance is strong；Bath stability is preferable；Plating speed is 18.7 μm/h；Good bonding strength；Brightness is good.
Chemical palladium-plating: by the substrate containing nickel coating, it is placed in progress chemical palladium-plating processing in chemical palladium plating solution, controls chemical plating
The pH of palladium liquid is that 5.5 temperature are 50 DEG C, and the time of chemical palladium-plating processing is 30min, the formula of chemical palladium plating solution are as follows: palladium nitrate
1.5g/L, sodium hypophosphite 10g/L, ethylenediamine 30g/L, triethanolamine 25g/L, citric acid 20g/L, ammonium citrate 8g/L, alkyl
Thiocarbamide 25mg/L, sodium thiosulfate 20mg/L.
Chemical gilding: by the substrate of nickeliferous palladium coating, progress chemical gilding processing, controlization in chemical gold plating liquid are placed in
It is 85 DEG C that the pH for learning gold plating liquid, which is 6.0 temperature, and the time of chemical gilding processing is 10min, the formula of chemical gold plating liquid are as follows: cyaniding
Golden potassium 3.0g/L, potassium hydroxide 100mL/L.
Product is put into the sink for filling clear water, sufficiently recycles the remaining gold-containing solution of plate face, then product is placed in temperature
Degree thoroughly removes the remaining medical fluid of plate face, obtains silver-based-NiPdAu route to carry out processing 2min in 60 DEG C of hot water.
Assessment of performance: 2 products obtained therefrom solderability of embodiment is strong, and weldability is good；Binding force is good, is measured using heating pulling method
Bond strength is 2978gf；Corrosion resistance is strong；With the copper-based pcb board ratio (thermal coefficient 16.5W/mK) of tradition, the thermally conductive system of product
Number is improved to 21.5W/mK, improves 30%, and thermal conductivity is high, and it is uniform to radiate.It can be perfectly suitable for heat-resisting to product, anti-corrosion
The equal higher field of performance requirements.
Embodiment 3
Cleaning: silver-based substrate is put into the super sink for filling ultrapure water, submerges silver-based substrate, is applied under room temperature light
Micro-vibration handles 10min, removes the impurity such as the dust of silver-based plate face.Product is put into the dodecyl sulphur of mass fraction 5% again
Sonic oscillation oil removal treatment is carried out in the mixed solution of sour sodium and 30g/L sodium hydroxide；Make 80g/L lauryl ammonium chloride with
30mL/L nitrate mixture sonic oscillation is carried out except oxide process.
Microetch processing: by the silver-based substrate of above-mentioned cleaned processing, 30mL/L containing methane sulfonic acid and potassium permanganate are placed in
Microetch processing is carried out in the mixed solution of 100g/L, treatment temperature is 25 DEG C, time 2min, after microetch processing, silver layer surface
It is smooth, it is smooth；Microetch uniform pore diameter is preferable, and surface roughness is small；Micro-etching speed is 1.25 μm/min, is met the requirements；Microetch
Liquid system is stablized, controllable-rate.
Pickling: the silver-based substrate handled through microetch is placed in the perchloric acid solution that concentration is 100mL/L, handles 2min.
Pre- pickling: by the perchloric acid solution that concentration is 10mL/L of being placed in through pickling processes, 2min is handled.
Palladium activation, the silver-based substrate that will be handled through pre- pickling are placed in perchloric acid containing 90mL/L and the perchloric acid of 80mL/L
In the palladium activating solution of palladium, in 25 DEG C, 2min is handled.
Pickling afterwards: the silver-based substrate that will be activated through palladium is placed in the perchloric acid solution that concentration is 20mL/L, processing
2min。
Chemical nickel plating: by the silver-based substrate that pickling is handled after, progress chemical nickel plating processing in chemical nickel-plating liquid, control are placed in
The pH of chemical nickel-plating liquid processed is 3.0, and temperature is 85 DEG C, and the time of chemical nickel plating processing is 25min, and the group of chemical nickel-plating liquid becomes
Nickel sulphonic acid 30g/L, sodium hypophosphite 30g/L, lactic acid 20g/L, propionic acid 10g/L, sodium citrate 12g/L, Potassiumiodate 45mg/L, PPS
8mg/L,DEP 8mg/L.Chemical Ni-plating layer is smooth；Porosity is low, and detection resulting value is 0.11/cm2, corrosion resistance of coating pole
By force；Bath stability is fabulous；Plating speed is 34.5 μm/h；Binding force is good；Brightness is good.
Chemical palladium-plating: by the substrate containing nickel coating, it is placed in progress chemical palladium-plating processing in chemical palladium plating solution, controls chemical plating
The pH of palladium liquid is that 6.5 temperature are 52 DEG C, and the time of chemical palladium-plating processing is 40min, the formula of chemical palladium plating solution are as follows: palladium nitrate
1.5g/L, sodium hypophosphite 12g/L, ethylenediamine 40g/L, triethanolamine 30g/L, citric acid 25g/L, ammonium citrate 12g/L, alkyl
Thiocarbamide 30mg/L, sodium thiosulfate 25mg/L.
Chemical gilding: by the substrate of nickeliferous palladium coating, progress chemical gilding processing, controlization in chemical gold plating liquid are placed in
It is 85 DEG C that the pH for learning gold plating liquid, which is 6.2 temperature, and the time of chemical gilding processing is 10min, the formula of chemical gold plating liquid are as follows: cyaniding
Golden potassium 3.0g/L, potassium hydroxide 100mL/L.
Product is put into the sink for filling clear water, sufficiently recycles the remaining gold-containing solution of plate face, then product is placed in temperature
Degree thoroughly removes the remaining medical fluid of plate face, obtains silver-based-NiPdAu route to carry out processing 3min in 65 DEG C of hot water.
Assessment of performance: 3 products obtained therefrom solderability of embodiment is strong, and weldability is good；Binding force is good, is measured using heating pulling method
Bond strength is 2954gf；Corrosion resistance is strong；With the copper-based pcb board ratio (thermal coefficient 16.5W/mK) of tradition, the thermally conductive system of product
Number is improved to 22.1W/mK, improves 34%, and thermal conductivity is high, and it is uniform to radiate.It can be perfectly suitable for heat-resisting to product, anti-corrosion
The equal higher field of performance requirements.
Embodiment 4
Other conditions are same as Example 3, and only micro-etching agent is the molten of 10mL/L containing methane sulfonic acid and potassium permanganate 60g/L
Liquid, after microetch processing, silver layer surface is smooth, smooth；Microetch uniform pore diameter is preferable, but hole depth is shallower, surface roughness compared with
It is small；Micro-etching speed is 0.50 μm/min, and rate is lower.
In the above various embodiments: before wiring board carries out microetch processing, needing successively to carry out hot water wash and double washings behaviour
Make.When hot water wash, treatment temperature is 55~65 DEG C, and the processing time is 1~3min, double washings for by product be placed in water flow it is lasting and
In uniform second level sink, 2~3min of processing is carried out, the remaining acidic materials of plate face, i.e. acidic cleaning are washed away.Wiring board into
It goes before pre- pickling processing, wiring board need to be carried out to double water washing operations, the processing time is 2~3min, before removing plate face is remaining
Set medical fluid.
After wiring board carries out before pickling processing, wiring board need to be carried out to double water washing operations, the processing time is 2~3min,
Remove the remaining preposition medical fluid of plate face.
Before wiring board carries out the processing of chemical nickel plating porpezite, wiring board need to carry out to double water washing operations, the processing time is 2~
3min removes the remaining preposition medical fluid of plate face.
When wiring board carries out Chemical nickel and palladium plating process processing, double washings twice need to be carried out, after being respectively chemical nickel plating,
After removing the remaining chemical nickel plating medical fluid of plate face and chemical palladium-plating, the remaining chemical palladium-plating medical fluid of plate face is removed.Handle the time
To be 2~3min.
Comparative example 1
Other conditions are same as Example 1, and only micro-etching agent is the solution of 30mL/L containing nitric acid and sodium peroxydisulfate 100g/L；Knot
After the processing of fruit microetch, there is white precipitate immediately in surface；Silver layer surface is concave-convex；Microetch pore size is different, and roughness is big, some
Microetch hole is also deposited covering；Micro-etching speed is big, but microetch system is unstable, and rate is uncontrollable.
Comparative example 2
Other conditions are same as Example 2, and only micro-etching agent is the solution of chloracid 30mL/L and iron chloride 100g/L, as a result
After microetch processing, silver layer surface is more smooth, more smooth；Microetch aperture is more uniform, and surface roughness is small；Micro-etching speed is smaller,
Microetch system is unstable, and rate is uncontrollable.
Comparative example 3
Other conditions are same as Example 3, and only micro-etching agent is the solution of 30mL/L containing perchloric acid and Na2Fe04 100g/L,
After microetch processing, silver layer surface is more smooth, more smooth；Microetch aperture is more uniform, and surface roughness is smaller；Micro-etching speed compared with
Greatly, microetch system is unstable, and rate is uncontrollable；It does not dry up and is placed in air after processing, microetch surface changes colour in 30s
Oxidative phenomena.
Comparative example 5
Other conditions are same as Example 1, only nickel-plating liquid from it is different, the plating in embodiment on silver-based substrate can not be obtained
Nickel effect, specific nickel-plating liquid composition and results of property are as shown in table 1:
1 nickel-plating liquid of table and results of property
The foregoing is merely the ideal examples of the present invention, are not intended to limit the invention.Technical scope of the invention
Content on not limited to this specification, all any modifications made within technical thought of the invention and principle are modified or are changed
Into should all be by protection of the invention.
Claims (10)
1. a kind of silver-based wiring board of chemical nickel plating porpezite, it is characterised in that: the silver-based wiring board includes silver-based substrate, described
The surface of silver-based substrate is successively plated with nickel layer, palladium layers, layer gold from the inside to the outside.
2. preparing a kind of method of the silver-based wiring board of chemical nickel plating porpezite as described in claim 1, which is characterized in that including
Following steps: before cleaned treated silver-based substrate successively carries out microetch, pickling, pre- pickling, palladium activation, rear pickling
Reason, then the silver-based substrate through pre-treatment is subjected to chemical nickel plating, chemical palladium-plating, chemical gilding successively up to the coating containing NiPdAu
Silver-based wiring board.
3. a kind of preparation method of the silver-based wiring board of chemical nickel plating porpezite according to claim 2, it is characterised in that: institute
Stating cleaning treatment process is, silver-based substrate is first cleaned 10~15min with ultrapure water, then carries out oil removal treatment again, except oxidation
Object processing；The oil removal treatment using mass fraction 3%~5% dodecyl sodium sulfate and 20~30g/L sodium hydroxide
Mixed solution, it is described except oxide process using at least one of the methane sulfonic acid of 30mL/L, chloric acid, perchloric acid, nitric acid with
The mixture of 50~80g/L lauryl ammonium chloride.
4. a kind of preparation method of the silver-based wiring board of chemical nickel plating porpezite according to claim 2, it is characterised in that: institute
Stating microetch process is, cleaned treated silver-based substrate is placed in by the mixed solution of oxide and microetch acid, in 20~
2~3min is handled at 30 DEG C；The concentration of the oxide is 60~120g/L, and the concentration of microetch acid is 15~40mL/L；It is described
Any one of oxide in potassium permanganate, hydrogen peroxide, the microetch acid is in nitric acid, chloric acid, methane sulfonic acid
Any one.
5. a kind of preparation method of the silver-based wiring board of chemical nickel plating porpezite according to claim 2, it is characterised in that: institute
State acid cleaning process are as follows: the silver-based substrate that will be handled through microetch is placed in the pickling solution that concentration is 80~120mL/L, processing 1~
3min；The pickling solution is selected from least one of nitric acid solution, solution chlorate, perchloric acid solution, methanesulfonic acid solution；
The pre- pickling process are as follows: by the silver-based substrate through pickling processes, be placed in the pre- pickling solutions that concentration is 6~12mL/L
In, handle 1~3min；The pre- pickling solutions are in nitric acid solution, solution chlorate, perchloric acid solution, methanesulfonic acid solution
At least one.
6. a kind of preparation method of the silver-based wiring board of chemical nickel plating porpezite according to claim 2, it is characterised in that: institute
State palladium activation process are as follows: the silver-based substrate that will be handled through pre- pickling is placed in palladium activating solution, in 20~30 DEG C, processing 2~
3min, the palladium activating solution are made of acid with the palladium salt of corresponding acid ion, and the acid is selected from nitric acid, chloric acid, perchloric acid or first
Base acid in any one；The concentration of the acid is 60~100mL/L；The concentration of the palladium salt of corresponding acid ion is 60~
120mL/L。
Pickling process after described are as follows: it is molten to be placed in the rear pickling that concentration is 15~40mL/L for the silver-based substrate that will be activated through palladium
In liquid, 1~3min is handled, the rear pickling solutions are selected from nitric acid solution, solution chlorate, perchloric acid solution, methanesulfonic acid solution
At least one of.
7. a kind of preparation method of the silver-based wiring board of chemical nickel plating porpezite according to claim 2, it is characterised in that: institute
State nickel process are as follows: by the silver-based substrate that pickling is handled after, be placed in progress chemical nickel plating processing in chemical nickel-plating liquid, control
The pH of chemical nickel-plating liquid processed is 3.0~4.5, and temperature is 85~90 DEG C, and the time of chemical nickel plating processing is 25~40min,
The chemical nickel-plating liquid includes following composition: 25~35g/L of nickel sulphonic acid, 20~40g/L of sodium hypophosphite, sodium citrate 10
~15g/L, 15~25g/L of lactic acid, 5~15g/L of propionic acid；35~50mg/L of Potassiumiodate, 5~10mg/L of PPS, DEP 5~
10mg/L。
8. a kind of preparation method of the silver-based wiring board of chemical nickel plating porpezite according to claim 2, it is characterised in that: institute
State chemical palladium-plating process are as follows: the silver-based substrate that will be handled through chemical nickel plating is placed in progress chemical palladium-plating processing in chemical palladium plating solution,
The pH for controlling chemical palladium plating solution is 4.5~6.5, and temperature is 48~52 DEG C, and the time of chemical palladium-plating processing is 25~40min.
9. a kind of preparation method of the silver-based wiring board of chemical nickel plating porpezite according to claim 8, it is characterised in that: institute
State chemical palladium plating solution include following composition: 1.2~1.5g/L of palladium nitrate, 8~12g/L of sodium hypophosphite, 25~40g/L of ethylenediamine,
Triethanolamine 20g~30g/L, 15~25g/L of citric acid, 6~12g/L of ammonium citrate, 20~30mg/L of alkyl thiourea, thio sulphur
Sour 15~25mg/L of sodium.
10. a kind of preparation method of the silver-based wiring board of chemical nickel plating porpezite according to claim 2, which is characterized in that
The chemical gilding process are as follows: the silver-based substrate that will be handled through chemical palladium-plating is placed in chemical gold plating liquid and carries out at chemical gilding
Reason, the pH for controlling chemical gold plating liquid is 5.8~6.2, and temperature is 82~85 DEG C, and the time of chemical gilding processing is 8~12min；
The chemical gold plating liquid includes following composition: 2.0~4.0g/L potassium auricyanide, 100~120mL/L potassium hydroxide.
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| CN116288289A (en) * | 2023-02-24 | 2023-06-23 | 江苏富乐华半导体科技股份有限公司 | Method for plating nickel and silver on ceramic copper-clad carrier plate |
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