CN104342644B - A kind of chemical plating liquid and silver-coating method - Google Patents
A kind of chemical plating liquid and silver-coating method Download PDFInfo
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- CN104342644B CN104342644B CN201310312530.5A CN201310312530A CN104342644B CN 104342644 B CN104342644 B CN 104342644B CN 201310312530 A CN201310312530 A CN 201310312530A CN 104342644 B CN104342644 B CN 104342644B
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- chemical
- plating liquid
- silver
- chemical plating
- liquid
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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
Abstract
The invention provides a kind of chemical plating liquid, the chemical plating liquid includes silver salt, complexing agent, pH adjusting agent, surfactant；The complexing agent includes ammonium citrate, ammonium sulfate and cysteine；The weight ratio of the ammonium citrate, ammonium sulfate and cysteine is 1：0.5‑1.5：0.002 0.02, the pH of the chemical plating liquid is 8.2 10.2.Method present invention also offers chemical silvering is carried out with the chemical plating liquid.The product appearance matter plated out with chemical plating liquid of the invention is close, uniformly, and the product that the similar silver plating liquid of in the market is plated out then outward appearance substantially has that the uneven particle of protrusion is even local plating leakage phenomenon occurs.And chemical plating liquid of the invention start decompose time it is longer compared with the resolving time of the similar silver plating liquid of in the market, it is more stable.
Description
Technical field
The invention belongs to chemical plating field, more particularly to a kind of chemical plating liquid and silver-coating method.
Background technology
The characteristics of there is good solderability, weatherability and electric conductivity due to silver, so using chemical silvering come to copper-based
The protection of material has been printed circuit-board industry and has widely used.At present, conventional copper-based chemical silvering has two methods：1st, aoxidize
The chemical silver impregnation method of reduction；2nd, displacement chemical silver plating method.Because redox is silver-plated, volume additional reducing agent is needed so that chemical silvering is molten
Liquid is easily unstable, and when using, in addition it is also necessary to it is sensitized pre-treatment accordingly to metal base, production cost is high, hinders
Its extensive use industrially, thus displacement chemical silver plating method is better than needing to use the redox chemistry of reducing agent silver-plated
Method.And, potassium cyanide is added in order to increase the stability of silver plating liquid, in some chemical silvering solution as complexing agent, potassium cyanide
There is severe toxicity, pollute environment.Displacement chemical silver plating method, the metal active using copper is stronger than silver, directly using copper as reducing agent, passes through
Copper realizes the directly silver-plated purpose in copper surface with the displacement reaction of silver ion.But similar liquid medicine product in the market is main
It is strong-acid type liquid medicine, its stronger acidity can corrode Copper base material, and its coating is coarse, it is impossible to meet the need of present electron trade
Will.
The Chinese patent of Publication No. CN101182637A discloses a kind of alkalescence chemical plating liquid, comprising following consumption
Component：Silver ion or silver-colored complex ion 0.01-20g/L, amine complexing agent 0.1-150g/L, amino acids complexing agent 0.1-
150g/L, polyhydroxy acids complexing agent 0.1-150g/L.The alkalescence chemical plating liquid stability is poor, and utilization rate is low, and coating holds
Oxidizable jaundice.
The content of the invention
A kind of present invention technical problem unstable to solve chemical plating liquid of the prior art, there is provided chemistry of stabilization
Silver plating liquid and its silver-coating method.
The invention provides a kind of chemical plating liquid, the chemical plating liquid includes silver salt, complexing agent, pH adjusting agent, surface
Activating agent；The complexing agent includes ammonium citrate, ammonium sulfate and cysteine；The ammonium citrate, ammonium sulfate and cysteine
Weight ratio be 1：0.5-1.5：0.002-0.02, the pH of the chemical plating liquid is 8.2-10.2.
Present invention also offers a kind of chemical silver plating method, the method includes being placed into workpiece to be plated in chemical plating liquid
Carry out chemical plating；Wherein, the chemical plating liquid is chemical plating liquid of the present invention.
Chemical plating liquid of the invention, ammonium citrate, ammonium sulfate, cysteine is suitable with the complexing power of silver ion, will
They are 1 according to the weight ratio of ammonium citrate, ammonium sulfate and cysteine：0.5-1.5：The ratio mixing of 0.002-0.02 is easy
There is symbiosis, generate mixing complex type, increase the stability of chemical plating liquid.
Brief description of the drawings
Fig. 1 is pattern photo of the plating silver products of embodiment 1 under 400 times of magnifying glasses；
Fig. 2 is pattern photo of the plating silver products of comparative example 1 under 400 times of magnifying glasses.
Specific embodiment
In order that technical problem solved by the invention, technical scheme and beneficial effect become more apparent, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention, is not intended to limit the present invention.
The invention provides a kind of chemical plating liquid, the chemical plating liquid includes silver salt, complexing agent, pH adjusting agent, surface
Activating agent；The complexing agent includes ammonium citrate, ammonium sulfate and cysteine；The ammonium citrate, ammonium sulfate and cysteine
Weight ratio be 1：0.5-1.5：0.002-0.02, the pH of the chemical plating liquid is 8.2-10.2.Complexing agent is maintained at above-mentioned
In the range of can keep the good stability of plating solution, make that plating is uniform, product bright property is good.
In the present invention, in order to obtain making the coating performance for obtaining good, it is preferable that the content of the silver salt is 0.5-5g/L,
The content of the complexing agent is 1-10g/L；The content of the surfactant is 13-30 ppm.
According to chemical plating liquid provided by the present invention, the silver salt, pH adjusting agent and surfactant are without special
Limitation, can be various silver salt commonly used in the art, pH adjusting agent and surfactant.In the present invention, the silver salt is nitric acid
At least one in silver, silver iodide and arachic acid silver；The pH adjusting agent be NaOH, potassium hydroxide and sulfuric acid in extremely
Few one kind；The surfactant is lauryl sodium sulfate, PEG-1000, PEG-300, neopelex and PEG-
At least one in 6000.
In the present invention, it is preferable that the chemical plating liquid also includes ceric sulfate, and the concentration of the ceric sulfate is 1-
10ppm.Also contain lanthana in the chemical plating liquid；The concentration of the lanthana is 5-50ppm.
The ceric sulfate can be co-deposited with silver coating, make coating finer and smoother, turn white.Lanthana effect is added simultaneously
More preferably.
In the present invention, the chemical plating liquid is also filed including the nitrogen of benzo three, and the concentration of the BTA is 0.2-
3ppm.The nitrogen of benzo three file can prevent from preventing silver layer oxidation to occur or corrodes in chemical plating.
Present invention also offers a kind of chemical silver plating method, the method includes being placed into workpiece to be plated in chemical plating liquid
Carry out chemical plating；Wherein, the chemical plating liquid is chemical plating liquid of the present invention.
In the present invention, workpiece to be plated can be the metal active metal stronger than silver, such as copper, nickel, iron and aluminium.
In order that chemical silvering effect is more preferable, it is preferable that the temperature of the chemical plating liquid is 41-48 DEG C, the chemistry
Silver-plated time 5-9min.
In order to preferably protect silver coating, it is preferable that the method is carried out at protection after being additionally included in chemical silvering to silver layer
The step of reason.The method of the protection treatment is to utilize BTA, tetrazole, and lauryl mercaptan forms complexing and protects with silver
Sheath, reaches protection silver coating purpose.
In order that silver coating to obtain adhesion more preferable, it is preferable that the method carries out pre-treatment before being additionally included in chemical silvering
The step of.The pre-treatment includes oil removing, acid etching.Will repeatedly be washed after oil removing and acid etching.
Chemical plating liquid of the invention and its chemical silver plating method are suitable for SBID（super beam induced
The super laser-induced depositions of deposition, are a kind of plastics composite and its surface selective metallization process.Specifically use
Energetic particle beam bombards material surface, restores metal crystal nuclei, and then the method for use electroless copper is bombarded in energetic particle beam
Layer of metal copper is plated at surface, then thickeies layers of copper to produce the technology of circuit board with traditional plating again）With LDS works
The 3D antenna for mobile phone of skill production and the silver-plated demand of Related product, because the chemical plating liquid belongs to alkalescent, it is to avoid acid is to copper facing
Line corrodes, and due to the weight of addition ammonium citrate, ammonium sulfate and cysteine, and ammonium citrate, ammonium sulfate and cysteine
Amount is than being 1：0.5-1.5：0.002-0.02, makes chemical plating liquid stabilization and silver-plated speed is fast, 5min can replacement ag plating 0.5 it is micro-
More than rice, the system of unused this complexing agent is 0.25 micron, and production efficiency is high.And chemical plating liquid displacement copper ion of the invention
Content can reach more than 3g/L, and more existing chemical plating liquid uses more convenient, chemical silvering higher to utilization rate of active components
Liquid is safeguarded more stable.
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1
Chemical plating liquid：Silver nitrate 0.5g/L；Ammonium citrate 0.5g/L；Ammonium sulfate 0.5g/L；Cysteine 1ppm；12
Sodium alkyl sulfate 3ppm；BTA 1ppm；PEG-1000 10ppm；With sodium hydroxide solution, pH value is reconciled for 9.0 obtain
Chemical plating liquid A1；
Chemical silvering：
1st, oil removing：Copper workpiece to be plated is carried out into ultrasonic oil removing；
2nd, acid etching：The workpiece dilute acid soln to be plated immersion that step 1 is obtained is except oxide layer；
3rd, chemical silvering：Chemical plating liquid A1 is heated to 45 DEG C, then the workpiece to be plated that step 2 is obtained is placed on and is added
9min is reacted in chemical plating liquid after heat；
4th, protection treatment：The plating piece that step 3 is obtained is placed on 3min is processed in silver protecting agent, then drying obtains silver-plated
Product S1.
Will repeatedly be washed between above step.
Embodiment 2
Chemical plating liquid：Silver nitrate 4g/L；Ammonium citrate 5g/L；Ammonium sulfate 2.5g/L；Cysteine 50ppm；Sulfuric acid is high
Cerium 1ppm；Lanthana 5ppm；Lauryl sodium sulfate 10ppm； PEG-300 40ppm；, with sodium hydroxide solution, reconcile pH
It is worth for 9.0 obtain chemical plating liquid A2；
Chemical silvering：
1st, oil removing：Copper workpiece to be plated is carried out into ultrasonic oil removing；
2nd, acid etching：The workpiece dilute acid soln to be plated immersion that step 1 is obtained is except oxide layer；
3rd, chemical silvering：Chemical plating liquid A2 is heated to 45 DEG C, then the workpiece to be plated that step 2 is obtained is placed on and is added
9min is reacted in chemical plating liquid after heat；
4th, protection treatment：The plating piece that step 3 is obtained is placed on 3min is processed in silver protecting agent, then drying obtains silver-plated
Product S2.
Will repeatedly be washed between above step.
Embodiment 3
Chemical plating liquid：Silver iodide 1g/L；Ammonium citrate 0.5g/L；Ammonium sulfate 0.75g/L；Cysteine 10ppm；Sulfuric acid
Cerium 5ppm high；Lanthana 50ppm；BTA 0.2ppm；Lauryl sodium sulfate 30ppm； PEG-6000 70ppm；With
Sodium hydroxide solution, reconciles pH value for 9.0 obtain chemical plating liquid A3；
Chemical silvering：
1st, oil removing：Copper workpiece to be plated is carried out into ultrasonic oil removing；
2nd, acid etching：The workpiece dilute acid soln to be plated immersion that step 1 is obtained is except oxide layer；
3rd, chemical silvering：Chemical plating liquid A3 is heated to 48 DEG C, then the workpiece to be plated that step 2 is obtained is placed on and is added
5min is reacted in chemical plating liquid after heat；
4th, protection treatment：The plating piece that step 3 is obtained is placed on 3min is processed in silver protecting agent, then drying obtains silver-plated
Product S3.
Will repeatedly be washed between above step.
Embodiment 4
Chemical plating liquid：Arachic acid silver 2g/L；Ammonium citrate 2g/L；Ammonium sulfate 2g/L；Cysteine 4ppm；Sulphur
Acid cerium 4ppm high；BTA 0.8ppm；Neopelex 12ppm； PEG-1000 40ppm；Use potassium hydroxide
Solution, reconciles pH value for 8.6 obtain chemical plating liquid A4；
Chemical silvering：
1st, oil removing：Copper workpiece to be plated is carried out into ultrasonic oil removing；
2nd, acid etching：The workpiece dilute acid soln to be plated immersion that step 1 is obtained is except oxide layer；
3rd, chemical silvering：Chemical plating liquid A4 is heated to 41 DEG C, then the workpiece to be plated that step 2 is obtained is placed on and is added
9min is reacted in chemical plating liquid after heat；
4th, protection treatment：The plating piece that step 3 is obtained is placed on 3min is processed in silver protecting agent, then drying obtains silver-plated
Product S4.
Will repeatedly be washed between above step.
Embodiment 5
Chemical plating liquid：Silver nitrate 5g/L；Ammonium citrate 5g/L；Ammonium sulfate 5g/L；Cys2 5ppm；Ceric sulfate
10ppm；Lanthana 30ppm；BTA 3ppm；Lauryl sodium sulfate 30ppm；PEG-1000 100ppm；, use hydrogen-oxygen
Change sodium solution, reconcile pH value for 8.6 obtain chemical plating liquid A5；
Chemical silvering：
1st, oil removing：Copper workpiece to be plated is carried out into ultrasonic oil removing；
2nd, acid etching：The workpiece dilute acid soln to be plated immersion that step 1 is obtained is except oxide layer；
3rd, chemical silvering：Chemical plating liquid A5 is heated to 45 DEG C, then the workpiece to be plated that step 2 is obtained is placed on and is added
7min is reacted in chemical plating liquid after heat；
4th, protection treatment：The plating piece that step 3 is obtained is placed on 3min is processed in silver protecting agent, then drying obtains silver-plated
Product S5.
Will repeatedly be washed between above step.
Comparative example 1
Chemical silvering is carried out using the chemical plating liquid and method of the embodiment 1 of CN101182637A, products C S1 is obtained.
Method of testing and data
1st, salt spray test
Neutral salt spray test condition：In salt-mist corrosion tester, with the salting liquid that sodium chloride content is 5 ± 1%：Temperature
At 35 DEG C, the collection liquid after spraying, pH value is 6.5 ~ 7.2.Allow to adjust pH value with the watery hydrochloric acid or NaOH after dilution.
35 DEG C of test space temperature；The continuous spray testing time is 48H；Then ordinary atmospheric conditions are returned in case, are protected after stabilization
Hold 2H.Carry out outward appearance detection.Standard：Non-corroding, discoloration, coating come off.The results are shown in Table 1.
2nd, product appearance
（1）Corresponding product is amplified to 400 times of patterns for observing its surface with optical loupes, 1 is the results are shown in Table.
The product appearance matter that the liquid medicine is plated out is close, uniformly, and the product that the similar liquid medicine of in the market is plated out then outward appearance substantially has
The uneven particle of protrusion is even local to there is plating leakage phenomenon.
（2）The products C S1 of the product S1 of embodiment and comparative example 1 is amplified to 400 times of observations with optical loupes, is seen
The surface topography of plating silver products is examined, and shoots the photo of the lower pattern respectively such as Fig. 1 and Fig. 2.
Table 1
From table 1 it follows that the salt spray resistance ratio of the plating silver products prepared with chemical plating liquid of the invention
The salt spray resistance of the plating silver products of comparative example is good, and the outward appearance of the plating silver products obtained with chemical plating liquid of the invention is caused
Close, uniformly, and the outward appearance of the plating silver products that comparative example is obtained substantially has that the uneven particle of protrusion is even local plating leakage is occurred and show
As.
From the contrast of Fig. 1 and Fig. 2 more it should be apparent that the outward appearance of the plating silver products of embodiment 1 is fine and close, uniformly；And
The silver-plated product appearance of comparative example 1 substantially has the uneven particle of protrusion even part plating leakage phenomenon occur.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (12)
1. a kind of chemical plating liquid, it is characterised in that the chemical plating liquid includes silver salt, complexing agent, pH adjusting agent, surface-active
Agent；The complexing agent includes ammonium citrate, ammonium sulfate and cysteine；The weight of the ammonium citrate, ammonium sulfate and cysteine
Amount is than being 1：0.5-1.5：0.002-0.02, the pH of the chemical plating liquid is 8.2-10.2.
2. chemical plating liquid as claimed in claim 1, it is characterised in that the content of the silver salt is 0.5-5g/L, the network
The content of mixture is 1-10g/L；The content of the surfactant is 13-130 ppm.
3. chemical plating liquid as claimed in claim 1, it is characterised in that the silver salt is silver nitrate, silver iodide and eicosane
At least one in sour silver；The pH adjusting agent be NaOH and potassium hydroxide in one or two；The surface-active
Agent is at least one in lauryl sodium sulfate, PEG-1000, PEG-300, neopelex and PEG-6000.
4. chemical plating liquid as claimed in claim 1, it is characterised in that the chemical plating liquid also includes ceric sulfate, institute
The concentration for stating ceric sulfate is 1-10ppm.
5. chemical plating liquid as claimed in claim 4, it is characterised in that also contain lanthana in the chemical plating liquid；Institute
The concentration for stating lanthana is 5-50ppm.
6. the chemical plating liquid as described in claim 1-4 any one, it is characterised in that the chemical plating liquid also includes benzene
And triazole, the concentration of the BTA is 0.2-3ppm.
7. a kind of chemical silver plating method, it is characterised in that the method includes being placed into workpiece to be plated in chemical plating liquid carrying out
Chemical plating；Wherein, the chemical plating liquid is the chemical plating liquid described in claim 1-6 any one.
8. chemical silver plating method according to claim 7, it is characterised in that the temperature of the chemical plating liquid is 41-48
DEG C, the time 5-9min of the chemical silvering.
9. chemical silver plating method according to claim 7, it is characterised in that the method is additionally included in after chemical silvering to silver
The step of layer carries out protection treatment.
10. chemical silver plating method according to claim 9, it is characterised in that the method for protection treatment is to utilize complexing agent
With silver-colored Absorptive complex wave, organic protective film is formed.
11. chemical silver plating methods according to claim 7, it is characterised in that before the method is additionally included in chemical silvering
The step of carrying out pre-treatment.
12. chemical silver plating methods according to claim 11, it is characterised in that the pre-treatment includes oil removing, acid etching.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310312530.5A CN104342644B (en) | 2013-07-23 | 2013-07-23 | A kind of chemical plating liquid and silver-coating method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310312530.5A CN104342644B (en) | 2013-07-23 | 2013-07-23 | A kind of chemical plating liquid and silver-coating method |
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| Publication Number | Publication Date |
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| CN104342644A CN104342644A (en) | 2015-02-11 |
| CN104342644B true CN104342644B (en) | 2017-05-31 |
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| CN106343816A (en) * | 2016-11-04 | 2017-01-25 | 东莞华南设计创新院 | Insect prevention tatami |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1495287A (en) * | 2002-08-30 | 2004-05-12 | 希普利公司 | Plating method |
| CN1982503A (en) * | 2005-12-05 | 2007-06-20 | 罗门哈斯电子材料有限公司 | Metallization of dielectrics |
| CN1989573A (en) * | 2004-08-05 | 2007-06-27 | 积水化学工业株式会社 | Conductive fine particle, method for producing conductive fine particle and electroless silver plating liquid |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002694B (en) * | 2010-12-14 | 2012-07-04 | 江西理工大学 | Method for preparing uniform silver conducting layer on surface of metal or nonmetal material |
| CN102321879A (en) * | 2011-06-16 | 2012-01-18 | 东华大学 | Method for improving appearance and conductive performance of conductive microspheres |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1495287A (en) * | 2002-08-30 | 2004-05-12 | 希普利公司 | Plating method |
| CN1989573A (en) * | 2004-08-05 | 2007-06-27 | 积水化学工业株式会社 | Conductive fine particle, method for producing conductive fine particle and electroless silver plating liquid |
| CN1982503A (en) * | 2005-12-05 | 2007-06-20 | 罗门哈斯电子材料有限公司 | Metallization of dielectrics |
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