CN106283134A - A kind of rare earth improves Brush Plating silver plating liquid and preparation technology thereof and using method - Google Patents
A kind of rare earth improves Brush Plating silver plating liquid and preparation technology thereof and using method Download PDFInfo
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- CN106283134A CN106283134A CN201610815581.3A CN201610815581A CN106283134A CN 106283134 A CN106283134 A CN 106283134A CN 201610815581 A CN201610815581 A CN 201610815581A CN 106283134 A CN106283134 A CN 106283134A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/46—Electroplating: Baths therefor from solutions of silver
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/20—Other heavy metals
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/04—Electroplating with moving electrodes
- C25D5/06—Brush or pad plating
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The present invention provides a kind of rare earth improvement Brush Plating silver plating liquid; including following component and mass concentration thereof: silver salt 10 30g/L; modifying agent rare earth cerous nitrate 0.1 2g/L; complexant sulfosalicylic acid 50 200g/L, imidazoles 50 200g/L; protective agent hexamethylenetetramine 0.01 1g/L; additive N; N dimethylformamide 0.01 1g/L, Polyethylene Glycol 1 30g/L, ammonia 10 50g/L; stabilizer ammonium acetate 10 40g/L, potassium pyrophosphate 5 30g/L, and to regulate the pH value of solution by dust technology or dilute sodium hydroxide be 6.8 7.2;Present invention also offers preparation technology and the using method of rare earth improvement Brush Plating silver plating liquid.The present invention uses the silver salt of low toxicity, rare earth modifying agent, complexant, protective agent etc. to mix, and for neutral non-cyanide plating silvering solution, raw material is easy to get, and preparation technology is simple;The products application of the present invention carries out Brush Plating on copper or copper alloy surface, and method is simple, and coating is stable.
Description
Technical field
The present invention relates to technical field of electrochemistry, be specifically related to a kind of rare earth improvement Brush Plating silver plating liquid and preparation technology thereof
And using method.
Background technology
DL/T486-2010 standard specifies, disconnecting switch and earthed switch contact surface must be silver-plated, and thickness of coating is not
Less than 20 microns, to obtain relatively low contact resistance, thus ensure good electric conductivity, require that silver coating has resistance to simultaneously
The performances such as erosion, wear-resisting and fastness.Technique of brush plating utilizes the plated pen (anode) being wrapped with the extraordinary plating solution of jacket dipping to fit in work
Part (negative electrode) plated position the formation coating that does relative motion, its maximum feature be deposition velocity be about 10 times of Common platings with
On.Some manufacturer uses the method for Silver Brush Plating to repair underproof isolation switch contact silver coating the most at the scene
Multiple, so that thickness conformance with standard requirement, and there is no concerned countries standard or industry standard at present and contact silver coating technique is entered
Row clear stipulaties.What is more important, although functional silver-plated along with electroplating technology is at electronic devices and components, quasiconductor and instrument instrument
Popularization and application in table and fast-developing, but cyanide is silver-plated is still that the most silver-plated main way at present because of its Inherent advantage
Footpath.This allows for hypotoxic non-cyanide silver coating correlation technique becomes study hotspot always.Therefore, to without cyanogen Brush Plating silver plating process
Carry out furtheing investigate and there is certain realistic meaning.
Non-cyanide silver coating has obtained the extensive concern of people very early, such as: thiosulfate is silver-plated, imino-diacetic ichthyodin
The silver plating process such as silver-plated, Nicotinic acid silver plating, potassium ferrocyanide are silver-plated are invented by people.But, compare still with cyaniding plant of silver
There is shortcomings: (1) bath stability sex chromosome mosaicism: the silver ion in plating solution can become simple substance, Jin Erying under sunlight irradiates
Ringing the concentration of silver ion in plating solution, some complexant also can affect plating solution character, such as fourth two phthalimide facile hydrolysis, etc.;(2) coating
Adhesion is poor, and coating is easy to foaming, crackle occurs: owing to silver-plated product is usually copper and copper alloy, due to the normal potential of copper
More negative than silver much, when copper and alloy plating piece thereof insert plating solution, i.e. it may happen that displacement reaction before being not powered on, on plating piece surface
Forming displacement silver layer, it is poor with the adhesion of plating piece matrix, and also has the cupra matter of part to pollute plating solution simultaneously, generally adopts
This problem is solved by methods such as pre-silver-plated, leaching silver or amalgamate.
It is apparent that Brush Plating silver plating process flow process also needs to improve coating performance by plating solution research further, logical
Before crossing the plating of specification matrix material, plating posttreatment technique improve plating piece homogeneity, the brush plating time needs further briefly to simplify
Application operating.
Summary of the invention
It is an object of the invention to provide a kind of rare earth improvement Brush Plating silver plating liquid and preparation technology thereof, use the silver of low toxicity
Salt, complexant, protective agent etc. mix, and for neutral non-cyanide plating silvering solution, raw material is easy to get, and preparation technology is simple.The present invention's is another
One purpose is to provide above-mentioned rare earth improvement Brush Plating silver plating liquid and carries out electric plating method on copper and/or copper alloy surface, should
Method is simple, and coating is stable.
To achieve these goals, the technical solution used in the present invention is as follows:
A kind of rare earth improvement Brush Plating silver plating liquid, including following component and mass concentration thereof: silver salt 10-30g/L, modifying agent
Rare earth cerous nitrate 0.1-2g/L, complexant sulfosalicylic acid 50-200g/L, imidazoles 50-200g/L, protective agent hexamethylenetetramine
0.01-1g/L, additive DMF 0.01-1g/L, Polyethylene Glycol 1-30g/L, ammonia 10-50g/L, stabilizer
Ammonium acetate 10-40g/L, potassium pyrophosphate 5-30g/L, and be 6.8-7.2 by dust technology or diluted sodium hydroxide solution regulation pH value.
According to above scheme, described silver salt is silver nitrate or pyrovinic acid silver.
The preparation technology of a kind of rare earth improvement Brush Plating silver plating liquid, comprises the steps:
(1) preparation modifying agent, complexant, protective agent, the mixed solution of stabilizer, and be sufficiently stirred for making to be uniformly dispersed;
(2), under stirring, additive DMF is joined in the mixed liquor of step (1);
(3), under stirring, silver salt is joined in the mixed liquor of step (2);
(4), under stirring, additives polyethylene glycol is joined in the mixed liquor of step (3);
(5), under stirring, additive ammonia is added to the mixed liquor of step (4);
(6) sucking filtration, dust technology or diluted sodium hydroxide solution regulation pH value, be aged to obtain product.
A kind of using method of rare earth improvement Brush Plating silver plating liquid, silver-plated for copper and/or copper alloy surface, including as follows
Step:
(1) silver-plated copper and/or Cu alloy material degreasing fluid oil removing will be treated, then after activating solution soaks, with described
Rare earth improvement Brush Plating silver plating liquid carries out Brush Plating;
(2) plating piece after Brush Plating is neutralized impregnation process in neutralizing impregnation liquid;
(3) with distilled water, plating piece is rinsed well.
According to above scheme, described degreasing fluid includes following component and mass concentration thereof: NaOH 8-12g/L, Na2CO350-
60g/L, Na3PO450-60g/L, Na2SiO35-10g/L。
According to above scheme, described activating solution includes following component and mass concentration thereof: H2SO420-60g/L, HNO340-
80g/L, temperature during described immersion is 30-50 DEG C.
According to above scheme, described Brush Plating condition is: operating temperature is 25 DEG C, and electric current density is 5-20A/m2, plating solution
PH value is 6.8-7.2, and the Brush Plating time is 0.5-1.5min, and anode electrode is high pure graphite electrode.
According to above scheme, described neutralization impregnation liquid includes following component and mass concentration thereof: Na2CO320-30g/L,
Na3PO430-40g/L。
The invention has the beneficial effects as follows:
(1) present invention uses rare earth cerous nitrate to make as silver plating liquid modifying agent, the compounding of protective agent, additive and stabilizer
Obtain Resisting Property of Brush Electroplating Coating appearance uniform fine and close, bright, without defects such as peeling, bubbling, speckles, brush plating effect under the conditions of identical Brush Plating
Fruit is substantially better than the silver plating liquid being not added with modifying agent;
(2) present invention is without pre-silver-plated, leaching silver or amalgamate, just can obtain combining stronger silvering, and silver-plated work
Skill specification, operating easy, the Brush Plating time only has 0.5-1.5 minute, while ensureing thickness of coating (more than 20 microns), has
Avoid the coating color problem brought due to long-time Brush Plating to effect;
(3) raw material sources of the Brush Plating silver plating liquid of the present invention are extensive, show at the interim plating solution of the tests of 10 months
Good stability;
(4) the Brush Plating silver plating liquid of the present invention is neutral non-cyanide plating silvering solution, and toxicity is low, meets the environmental requirement of increasingly stringent
With cleaning production requirement.
Accompanying drawing explanation
Fig. 1 is the coating surface microscopic appearance schematic diagram of embodiment 1 center brush plating;
Fig. 2 is the coating surface microscopic appearance schematic diagram of embodiment 3 center brush plating;
Fig. 3 is the coating tangent plane microscopic appearance schematic diagram of embodiment 1 center brush plating;
Fig. 4 is the coating tangent plane microscopic appearance schematic diagram of embodiment 3 center brush plating.
Detailed description of the invention
With embodiment, technical scheme is illustrated below in conjunction with the accompanying drawings.
Embodiment 1:
The present invention provides a kind of rare earth improvement Brush Plating silver plating liquid, including following component and mass concentration thereof: silver nitrate
15g/L, modifying agent rare earth cerous nitrate 1g/L, complexant sulfosalicylic acid 150g/L, imidazoles 100g/L, protective agent six methine four
Amine 0.5g/L, additive DMF 0.05g/L, Polyethylene Glycol 10g/L, ammonia 20g/L, stabilizer ammonium acetate
30g/L, potassium pyrophosphate 15g/L, and be 7.1 by diluted sodium hydroxide solution regulation pH value.
The present invention provides a kind of rare earth improvement Brush Plating silver plating liquid, and preparation process comprises the steps:
(1) preparation modifying agent, complexant, protective agent, the mixed solution of stabilizer, and be sufficiently stirred for making to be uniformly dispersed;
(2), under stirring, DMF is joined in the mixed liquor of step (1);
(3), under stirring, silver salt is joined in the mixed liquor of step (2);
(4), under stirring, Polyethylene Glycol is joined in the mixed liquor of step (3);
(5), under stirring, ammonia is added to the mixed liquor of step (4);
(6) sucking filtration, regulate pH value with diluted sodium hydroxide solution, be aged to obtain product.
The present invention also provides for the using method of a kind of rare earth improvement Brush Plating silver plating liquid, for copper sheet electroplate, including
Following steps:
(1) silver-plated copper sheet degreasing fluid oil removing will be treated, then after activating solution soaks, carry out Brush Plating with silver plating liquid,
Brush Plating condition is: operating temperature is 25 DEG C, and electric current density is 5-20A/m2, bath pH value is 7.1, and the Brush Plating time is
1min, anode electrode is high pure graphite electrode;
(2) copper sheet after Brush Plating is neutralized impregnation process in neutralizing impregnation liquid;
(3) with distilled water, copper sheet is rinsed well.
Further, described degreasing fluid includes following component and mass concentration thereof: NaOH 9g/L, Na2CO350g/L,
Na3PO450g/L, Na2SiO39g/L;Described activating solution includes following component and mass concentration thereof: H2SO430g/L, HNO3
50g/L, temperature during described immersion is 40 DEG C;Described neutralization impregnation liquid includes following component and mass concentration thereof: Na2CO3
28g/L, Na3PO4 36g/L。
In order to contrast with the present invention, also make the Brush Plating silver plating liquid of a kind of modifying agent without rare earth, except not containing
Outside modifying agent rare earth cerous nitrate, remaining component and phase mass concentration are the most same as in Example 1, and preparation technology is the most equal with application process
With embodiment 1.
Use Japan's JSM-6510 type scanning electron microscope, coating and the Comparison study silver plating liquid to application the present embodiment product
Coating carries out microscopic appearance test, and result is shown in accompanying drawing 1 to accompanying drawing 4.Contrast accompanying drawing 1 and accompanying drawing 2 are it should be apparent that add
Deposit appearance (accompanying drawing 1) light of rare earth modifying agent is smooth, no significant defect, crystallize careful closely, crystal grain uniformly, porosity
Little, show that rare earth modifying agent improves the cathodic polarization of bath system, make crystallite dimension reduce, thus obtain the silver of dense uniform
Coating.And the thickness of coating uniformly (accompanying drawing 3), (silver coating thickness is not less than 20 to reach the regulation of DL/T486-2010 standard
Micron), it is better than not adding the thickness of coating (accompanying drawing 4) of the contrast silver plating liquid of rare earth modifying agent.
Embodiment 2:
The present invention provides a kind of rare earth improvement Brush Plating silver plating liquid, including following component and mass concentration thereof: silver nitrate
16g/L, modifying agent rare earth cerous nitrate 1.2g/L, complexant sulfosalicylic acid 140g/L, imidazoles 110g/L, protective agent six methine
Tetramine 0.6g/L, additive DMF 0.07g/L, Polyethylene Glycol 12g/L, ammonia 18g/L, stabilizer ammonium acetate
28g/L, potassium pyrophosphate 17g/L, and to regulate the pH value of solution by dust technology and dilute sodium hydroxide be 6.9.
The preparation technology of the present embodiment and application process are all with embodiment 1.
Placing (temperature 20-30 DEG C) through long sealing and standing, test the present embodiment product was at 0 month, 5 respectively
When the moon, 10 months shelf lifes, the coating performance obtained after plating, numbered No. 1-3 of coating.Use Japan's JSM-6510 type scanning
Electronic Speculum test thickness of coating;Use Germany's FISHER HM2000 type nano hardness work station test coating hardness;Coating and base material
Adhesion test utilizes method of scoring to carry out by GB/T 5270-2005: use the converted steel of 30 ° of sharp swords to draw cutter every in sample surface
Being mutually perpendicular to groove every 1mm, groove is divided into grid square, ensures a groove during line, and the cover layer observed in this region is
No peeling from Copper substrate;Utilize three-electrode system to investigate the corrosion resistance of silvering, investigate coating by the test of polarization curve
Corrosion resistance in sodium chloride solution.In three-electrode system, Electrode is coating sample, and auxiliary electrode takes platinum electrode, reference
Electrode is saturated calomel electrode, and test apparatus uses Holland's Autolab electrochemical workstation, test result such as following table:
Test result shows, the silver plating liquid that the present embodiment prepares is interim the standing of 10 months, the Brush Plating plating obtained
Layer stable performance.
Above example is only in order to illustrative not limiting technical scheme, although the present invention is entered by above-described embodiment
Gone detailed description, the person skilled of this area it is understood that the present invention can be modified or replaces on an equal basis, but
Any amendment and local without departing from spirit and scope of the invention are replaced and all should be contained in scope of the presently claimed invention.
Claims (8)
1. rare earth improvement Brush Plating silver plating liquid, it is characterised in that include following component and mass concentration thereof: silver salt 10-
30g/L, modifying agent rare earth cerous nitrate 0.1-2g/L, complexant sulfosalicylic acid 50-200g/L, imidazoles 50-200g/L, protective agent
Hexamethylenetetramine 0.01-1g/L, additive DMF 0.01-1g/L, Polyethylene Glycol 1-30g/L, ammonia 10-
50g/L, stabilizer ammonium acetate 10-40g/L, potassium pyrophosphate 5-30g/L, and by dust technology or diluted sodium hydroxide solution regulation pH
Value is 6.8-7.2.
Rare earth the most according to claim 1 improvement Brush Plating silver plating liquid, it is characterised in that described silver salt is silver nitrate or first
Base sulfonic acid silver.
3. the preparation technology of a rare earth improvement Brush Plating silver plating liquid, it is characterised in that comprise the steps:
(1) preparation modifying agent, complexant, protective agent, the mixed solution of stabilizer, and be sufficiently stirred for making to be uniformly dispersed;
(2), under stirring, additive DMF is joined in the mixed liquor of step (1);
(3), under stirring, silver salt is joined in the mixed liquor of step (2);
(4), under stirring, additives polyethylene glycol is joined in the mixed liquor of step (3);
(5), under stirring, additive ammonia is added to the mixed liquor of step (4);
(6) sucking filtration, regulates pH value with dust technology or diluted sodium hydroxide solution, is aged to obtain product.
Rare earth the most according to claim 1 improvement Brush Plating silver plating liquid using method, it is characterised in that for copper and/
Or copper alloy surface is silver-plated, comprises the steps:
(1) silver-plated copper and/or Cu alloy material degreasing fluid oil removing will be treated, then after activating solution soaks, use described rare earth
Improvement Brush Plating silver plating liquid carries out Brush Plating;
(2) plating piece after Brush Plating is neutralized impregnation process in neutralizing impregnation liquid;
(3) with distilled water, plating piece is rinsed well.
The using method of rare earth the most according to claim 4 improvement Brush Plating silver plating liquid, it is characterised in that described degreasing fluid
Including following component and mass concentration thereof: NaOH 8-12g/L, Na2CO350-60g/L, Na3PO450-60g/L, Na2SiO3
5-10g/L。
The neutral using method without cyanogen Brush Plating silver plating liquid the most according to claim 4, it is characterised in that described activating solution
Including following component and mass concentration thereof: H2SO420-60g/L, HNO340-80g/L, temperature during described immersion is 30-50
℃。
The neutral using method without cyanogen Brush Plating silver plating liquid the most according to claim 4, it is characterised in that described Brush Plating
Condition is: operating temperature is 25 DEG C, and electric current density is 5-20A/m2, bath pH value is 6.8-7.2, and the Brush Plating time is 0.5-
1.5min, anode electrode is high pure graphite electrode.
The neutral using method without cyanogen Brush Plating silver plating liquid the most according to claim 4, it is characterised in that described neutralization is soaked
Stain liquid includes following component and mass concentration thereof: Na2CO320-30g/L, Na3PO430-40g/L。
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Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108360000A (en) * | 2018-04-17 | 2018-08-03 | 江苏江润铜业有限公司 | Lian Lalian plates aqueous annealing liquid |
CN108716012A (en) * | 2018-06-25 | 2018-10-30 | 国网湖北省电力有限公司孝感供电公司 | Technique of brush plating method and coating and application |
CN109023450A (en) * | 2018-09-27 | 2018-12-18 | 南京市产品质量监督检验院 | A kind of sulfosalicylic acid plating silver additive, preparation method and the electroplate liquid comprising it |
CN109487308A (en) * | 2018-12-11 | 2019-03-19 | 湖北工程学院 | The method of neutral tin plating electrolyte and preparation method thereof and copper-based material surface tinning |
CN109504990A (en) * | 2018-12-11 | 2019-03-22 | 湖北工程学院 | A kind of weakly acidic pH Brush Plating silver plating liquid and its preparation process, application method |
CN109504989A (en) * | 2018-12-11 | 2019-03-22 | 湖北工程学院 | A kind of bright brush plating silver plating liquid and its preparation process, application method |
CN110528031A (en) * | 2019-08-06 | 2019-12-03 | 国网山东省电力公司电力科学研究院 | Based on the more first coordination systems of EDTA without cyanogen brush plating liquor and preparation method thereof |
CN111235608A (en) * | 2020-03-10 | 2020-06-05 | 国网浙江省电力有限公司电力科学研究院 | Cyanide-free silver-based composite plating solution, silver-based composite plating layer and preparation method thereof |
CN111235609A (en) * | 2020-03-10 | 2020-06-05 | 国网浙江省电力有限公司电力科学研究院 | Cyanide-free silver plating solution, silver plating layer and preparation method thereof |
CN112746295A (en) * | 2020-12-30 | 2021-05-04 | 苏州禾川化学技术服务有限公司 | Silver plating solution and ceramic surface silver plating method |
CN113416989A (en) * | 2021-06-25 | 2021-09-21 | 苏州瑞港环保科技有限公司 | Silver plating process and silver plated part |
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WO2024104283A1 (en) * | 2022-11-18 | 2024-05-23 | 温州泰钰新材料科技有限公司 | Composite plating solution, preparation method for composite coating, and electric contact material. |
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CN108716012A (en) * | 2018-06-25 | 2018-10-30 | 国网湖北省电力有限公司孝感供电公司 | Technique of brush plating method and coating and application |
CN109023450A (en) * | 2018-09-27 | 2018-12-18 | 南京市产品质量监督检验院 | A kind of sulfosalicylic acid plating silver additive, preparation method and the electroplate liquid comprising it |
CN109023450B (en) * | 2018-09-27 | 2020-06-16 | 南京市产品质量监督检验院 | Sulfosalicylic acid silver plating additive, preparation method thereof and electroplating solution containing sulfosalicylic acid silver plating additive |
CN109487308A (en) * | 2018-12-11 | 2019-03-19 | 湖北工程学院 | The method of neutral tin plating electrolyte and preparation method thereof and copper-based material surface tinning |
CN109504990A (en) * | 2018-12-11 | 2019-03-22 | 湖北工程学院 | A kind of weakly acidic pH Brush Plating silver plating liquid and its preparation process, application method |
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