CN108425137A - A kind of method that electro-deposition prepares silver-nickel electrical contact - Google Patents
A kind of method that electro-deposition prepares silver-nickel electrical contact Download PDFInfo
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- CN108425137A CN108425137A CN201810244363.8A CN201810244363A CN108425137A CN 108425137 A CN108425137 A CN 108425137A CN 201810244363 A CN201810244363 A CN 201810244363A CN 108425137 A CN108425137 A CN 108425137A
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- silver
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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
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
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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
Abstract
A kind of method that electro-deposition prepares silver-nickel electrical contact, belongs to the electroplating technology of material surface engineering.This method is：Choline chloride and ethylene glycol heating stirring are mixed, silver nitrate is added to being completely dissolved, is added nickel chloride, continuous heating stirs to solution that be presented dark green transparent, obtains electroplate liquid；DC electrodeposition is carried out to pretreated metallic matrix, obtains silver-nickel electrical contact；In electrodeposition process, the temperature of electroplate liquid is 30~50 DEG C, current density 1A/dm2~2A/dm2.This method is a kind of green method without cyanide electroplating silver-nickel, even if, it has used organic matter to make basal liquid in the method and has carried out electro-deposition, compared to cyanide electroplating method, this method is also improved in terms of environmental protection, and this method eliminates the phenomenon that traditional aqueous solvent generates hydrogen embrittlement in plating.This method be it is a kind of prepare it is simple, it is easy to operate, and the process of Sulfur tolerance and the good coating of electric conductivity can be obtained.
Description
Technical field
The present invention relates to a kind of methods that electro-deposition prepares silver-nickel electrical contact, belong to the plating skill of material surface engineering
Art field.
Background technology
Silver is the metal of generally acknowledged good conductivity, and silver can be effectively improved to the electric conductivity of metallic matrix, but silver as coating
Metal is more expensive to be unfavorable for industrial production, and the corrosion resistance of silvering is not high, in many electrical contacts application, it is desirable that material should
Having good electric conductivity again has good corrosion resistance, therefore, other a certain amount of metals is added in silvering, forms silver and close
Gold so that the existing good electric conductivity of coating has good Sulfur tolerance again.
Silver-nickel (Ag-Ni alloys) has good electric conductivity and thermal conductivity, and because the addition of nickel makes the resistance to of coating
Corrosion is improved, and silver-nickel is applied mostly on the contact head of low-voltage electrical apparatus, is such as switched, relay etc..The country is to silver-colored nickel
The research of alloy is simultaneously few, and the method also disunity prepared.Currently, based on electrosilvering mainly plates with cyaniding, because of cyanating solution
Stability is high, and current efficiency is high, and obtained coating light is good and is used, but cyanide has severe toxicity, endangers the mankind and nature
It is larger, therefore, seek a kind of green, the method plating Ag-Ni alloys of stability and high efficiency are necessary.
When Ag-Ni alloys being electroplated in traditional aqueous solution, due to there is hydrionic presence in water so that kept away in plating
Hydrogen embrittlement easily occurs for unavoidable evolving hydrogen reaction, the coating caused.Meanwhile a large amount of water being added when preparing electroplate liquid, to current
The situation of shortage of water resources is more unfavorable.
Invention content
The object of the present invention is to provide a kind of method that electro-deposition prepares silver-nickel electrical contact, this method is that one kind is not necessarily to
The green method of cyanide electroplating silver-nickel, even if having used organic matter to make basal liquid in the method and having carried out electro-deposition, compared
In cyanide electroplating method, this method is also improved in terms of environmental protection, and this method eliminates traditional aqueous solvent and produced in plating
The phenomenon that raw hydrogen embrittlement.This method is a kind of to prepare simple, technique easy to operate, and can obtaining Sulfur tolerance and the good coating of electric conductivity
Method.
Technical scheme is as follows：
The method that a kind of electro-deposition of the present invention prepares silver-nickel electrical contact, comprises the following steps that：
Step 1, metallic matrix pre-treatment
Metallic matrix is polished, oil removing, acid etching, obtain pretreated metallic matrix；
Step 2, electroplate liquid is prepared
Choline chloride and ethylene glycol are mixed, heating stirring, until solution is in colourless transparent liquid, obtains choline chloride-
Ethylene glycol eutectic solvent；Wherein, in molar ratio, choline chloride：Ethylene glycol=1：(1.5~3)；
Into choline chloride-ethylene glycol eutectic solvent, silver nitrate is added, it is complete to particles of silver nitrate to continue heating stirring
Dissolving, is then added nickel chloride, and continuous heating stirs to solution that be presented dark green transparent, obtains electroplate liquid；Wherein, by solid-to-liquid ratio
(unit g/L), silver nitrate：Choline chloride-ethylene glycol eutectic solvent=(30~80)：1, by solid-to-liquid ratio (unit g/L),
Nickel chloride：Choline chloride-ethylene glycol eutectic solvent=(20~40)：1；
Step 3, it is electroplated
Using above-mentioned electroplate liquid, DC electrodeposition is carried out to pretreated metallic matrix, obtains the silver-colored nickel on metallic matrix
Alloy, after cleaning, drying, as silver-nickel electrical contact；Wherein, in electrodeposition process, the temperature of electroplate liquid is 30~50 DEG C,
Current density is 1A/dm2~2A/dm2。
In the step 1, the metallic matrix, metal is carbon steel, low-alloy steel, copper, copper alloy, nickel or nickel alloy
In one kind.
In the step 1, the metallic matrix needs setting structure according to product.
In the step 1, the polishing, specially：The sand paper that metallic matrix is used to different model respectively, according to
Sequential processes metal base surface from thick to thin obtains the smooth metallic matrix without apparent cut in surface.
In the step 1, the oil removing, specially：The smooth metallic matrix without apparent cut in surface is used into alkali
Property mixed solution impregnated, soaking time be 60~90 DEG C, impregnate 10~30min after, be rinsed, obtained with deionized water
Metallic matrix after oil removing.
In the step 1, the acid etching, specially：It is 1 that metallic matrix after oil removing, which is placed in molar concentration,
In the hydrochloric acid solution of~2mol/L, acid etching is carried out, 1~2min is handled at 40~50 DEG C, is rinsed, is obtained with deionized water
To pretreated metallic matrix.
In the step 2, the heating stirring, heating temperature is 30~50 DEG C.
In the step 2, preferably, by solid-to-liquid ratio (unit g/L), silver nitrate：Choline chloride-ethylene glycol is low total
Molten solvent=(34~51)：1.
In the step 3, electrode system used is two electrode systems.
The silver-nickel being electrodeposited on metallic matrix prepared by method made above is touched as silver-nickel electricity
Head, in silver-nickel electrical contact, the thickness of silver-nickel coating is 5~8 μm, and Sulfur tolerance survey is carried out to silver-nickel electrical contact
Examination, corrosion resistance to sulfuric acid dew point result are 0.01157~0.17361mg/cm2H, silver-nickel in silver-nickel electrical contact
Plating layer resistivity is 0.001 Ω m-0.002 Ω m, and Sulfur tolerance test result is non-discolouring after immersing 30 minutes.
The method that a kind of electro-deposition of the present invention prepares silver-nickel electrical contact, advantage are：
1. this method electroplate liquid prepares simple, and cyanide electroplating is not used, is a kind of to realize economical and practical and environmentally friendly side
Method eliminates method of traditional water as solvent, eliminates evolving hydrogen reaction, reduces the negative shadow that hydrogen embrittlement brings coating
It rings.
2. by a process for preparing silver-colored nickel coating have good electric conductivity, resistance to sulfuric acid dew point corrosion and resistant to sulfur
Property.
Specific implementation mode
With reference to specific embodiment, the present invention is furture elucidated, it should be understood that and these embodiments are merely to illustrate the present invention,
Rather than it limits the scope of the invention.After having read the present invention, various equivalences of the those skilled in the art to the present invention
The modification of form falls within the application range as defined in the appended claims.
Following embodiment, removes specified otherwise, and the raw material and equipment of use are all from purchased in market.
Following embodiment prepares the shape and size of the metallic matrix used in silver-nickel electrical contact according to national standards
It is prepared by GB/T5587-2016；The silver-nickel corrosion resistance to sulfuric acid dew point test of preparation is carried out with reference to GBT28907-2012；
The silver-nickel Sulfur tolerance test method of preparation is as follows：The silver-nickel of preparation is immersed into the Na that mass percentage concentration is 1%2S
Solution, Na2S is that chemistry is pure.Solution temperature is 15~20 DEG C, and it is 30 minutes to immerse the time.The silver-colored nickel of observation is taken out after experiment
Whether alloy surface changes colour.
Embodiment 1
A kind of method that electro-deposition prepares silver-nickel electrical contact, comprises the following steps that：
Step 1, metallic matrix pre-treatment
Copper substrate is polished using sand paper, obtains the smooth Copper substrate without apparent cut in surface；
The smooth Copper substrate without apparent cut in surface is subjected to immersion oil removing, soaking time 80 using alkaline mixed solution
DEG C, after impregnating 20min, it is rinsed with deionized water, obtains the Copper substrate after oil removing；
Copper substrate after oil removing is placed in the hydrochloric acid solution that molar concentration is 1mol/L, acid etching is carried out, at 50 DEG C
1min is handled, is rinsed with deionized water, obtains pretreated Copper substrate；
Step 2, electroplate liquid is prepared
35g choline chlorides (ChCl) and 31g ethylene glycol (EG) are mixed, heating stirring, until solution is in water white transparency liquid
Body obtains choline chloride-ethylene glycol eutectic solvent；
Into choline chloride-ethylene glycol eutectic solvent, 2g silver nitrates are added, it is complete to particles of silver nitrate to continue heating stirring
Then 1.6g NiCl are added in fully dissolved2·6H2O, continuous heating stir to solution present dark green it is transparent, obtain 40mL plating
Liquid；During above-mentioned preparation electroplate liquid, heating stirring, heating and temperature control is 30~50 DEG C.
Step 3, it is electroplated
Cathode is used copper as using rhodium titanium alloy as insoluble anode using above-mentioned electroplate liquid, to pretreated gold
Belonging to matrix and carries out DC electrodeposition, electroplating time 1h obtains the silver-nickel on Copper substrate, is cleaned with deionized water, dries,
As silver-nickel electrical contact；Wherein, in electrodeposition process, the temperature control of electroplate liquid is 30~50 DEG C, current density 2A/
dm2。
Silver-nickel electrical contact manufactured in the present embodiment to be tested, wherein the thickness of silver-nickel coating is 7 μm,
Wherein, in silver-nickel, silver-colored mass percentage is 33.47wt%, and Sulfur tolerance test is carried out to silver-nickel electrical contact, resistance to
Corrosion of sulfuric acid at dew point results of property is 0.01157mg/cm2H, silver-nickel plating layer resistivity is in silver-nickel electrical contact
0.001 Ω m-0.002 Ω m, Sulfur tolerance test result are non-discolouring after immersing 30 minutes.
Embodiment 2
A kind of method that electro-deposition prepares silver-nickel electrical contact, comprises the following steps that：
Step 1, metallic matrix pre-treatment
Plain steel is polished using sand paper, obtains the smooth plain steel without apparent cut in surface；
The smooth plain steel without apparent cut in surface is subjected to immersion oil removing using alkaline mixed solution, soaking time is
It 80 DEG C, after impregnating 20min, is rinsed with deionized water, obtains the plain steel after oil removing；
Plain steel after oil removing is placed in the hydrochloric acid solution that molar concentration is 2mol/L, acid etching is carried out, 40
DEG C processing 2min, be rinsed with deionized water, obtain pretreated plain steel；
Step 2, electroplate liquid is prepared
75g choline chlorides (ChCl) and 95g ethylene glycol (EG) are mixed, heating stirring, until solution is in water white transparency liquid
Body obtains choline chloride-ethylene glycol eutectic solvent；
Into choline chloride-ethylene glycol eutectic solvent, 7.5g silver nitrates are added, continue heating stirring to particles of silver nitrate
It is completely dissolved, 3g NiCl is then added2·6H2O, continuous heating stir to solution present dark green it is transparent, obtain 100mL plating
Liquid；During above-mentioned preparation electroplate liquid, heating stirring, heating and temperature control is 30~50 DEG C.
Step 3, it is electroplated
Using above-mentioned electroplate liquid, using rhodium titanium alloy as insoluble anode, using carbon steel as cathode, to pretreated
Metallic matrix carries out DC electrodeposition, and electroplating time 1h obtains the silver-nickel on plain steel, cleaned with deionized water,
Drying, as silver-nickel electrical contact；Wherein, in electrodeposition process, the temperature control of electroplate liquid is 30~50 DEG C, current density
For 1.5A/dm2。
Silver-nickel electrical contact manufactured in the present embodiment to be tested, wherein the thickness of silver-nickel coating is 7 μm,
Wherein, in silver-nickel, silver-colored mass percentage is 50.51wt.%, and Sulfur tolerance test is carried out to silver-nickel electrical contact,
Corrosion resistance to sulfuric acid dew point result is 0.17361mg/cm2H, silver-nickel plating layer resistivity is in silver-nickel electrical contact
0.001 Ω m-0.002 Ω m, Sulfur tolerance test result are non-discolouring after immersing 30 minutes.
Embodiment 3
A kind of method that electro-deposition prepares silver-nickel electrical contact, comprises the following steps that：
Step 1, metallic matrix pre-treatment
Ni substrate is polished using sand paper, obtains the smooth Ni substrate without apparent cut in surface；
The smooth Ni substrate without apparent cut in surface is subjected to immersion oil removing, soaking time 80 using alkaline mixed solution
DEG C, after impregnating 20min, it is rinsed with deionized water, obtains the Ni substrate after oil removing；
Ni substrate after oil removing is placed in the hydrochloric acid solution that molar concentration is 1.5mol/L, acid etching is carried out, 40
DEG C processing 2min, be rinsed with deionized water, obtain pretreated Ni substrate；
Step 2, electroplate liquid is prepared
185g choline chlorides (ChCl) and 140g ethylene glycol (EG) are mixed, heating stirring, until solution is in water white transparency
Liquid obtains choline chloride-ethylene glycol eutectic solvent；
Into choline chloride-ethylene glycol eutectic solvent, 9g silver nitrates are added, it is complete to particles of silver nitrate to continue heating stirring
Then 4g NiCl are added in fully dissolved2·6H2O, continuous heating stir to solution present dark green it is transparent, obtain 200mL plating
Liquid；During above-mentioned preparation electroplate liquid, heating stirring, heating and temperature control is 30~50 DEG C.
Step 3, it is electroplated
Using above-mentioned electroplate liquid, using rhodium titanium alloy as insoluble anode, using nickel as cathode, to pretreated gold
Belonging to matrix and carries out DC electrodeposition, electroplating time 1h obtains the silver-nickel on Ni substrate, is cleaned with deionized water, dries,
As silver-nickel electrical contact；Wherein, in electrodeposition process, the temperature control of electroplate liquid is 30~50 DEG C, current density 1A/
dm2。
Silver-nickel electrical contact manufactured in the present embodiment to be tested, wherein the thickness of silver-nickel coating is 8 μm,
Wherein, in silver-nickel, silver-colored mass percentage is 20.79wt.%, and Sulfur tolerance test is carried out to silver-nickel electrical contact,
Corrosion resistance to sulfuric acid dew point result is 0.05556mg/cm2H, silver-nickel plating layer resistivity is in silver-nickel electrical contact
0.001 Ω m-0.002 Ω m, Sulfur tolerance test result are non-discolouring after immersing 30 minutes.
Embodiment 4
A kind of method that electro-deposition prepares silver-nickel electrical contact, with embodiment 1, the difference is that, metal used
Matrix is copper-tungsten, wherein in copper-tungsten, the mass percent of copper is 25wt%.
Silver-nickel electrical contact manufactured in the present embodiment to be tested, wherein the thickness of silver-nickel coating is 5 μm,
Wherein, in silver-nickel, silver-colored mass percentage is 53.08wt.%, and Sulfur tolerance test is carried out to silver-nickel electrical contact,
Corrosion resistance to sulfuric acid dew point result is 0.03507mg/cm2H, silver-nickel plating layer resistivity is in silver-nickel electrical contact
0.001 Ω m-0.002 Ω m, Sulfur tolerance test result are non-discolouring after immersing 30 minutes.
Embodiment 5
A kind of method that electro-deposition prepares silver-nickel electrical contact, with embodiment 2, the difference is that, metal used
Matrix is corronil, wherein in corronil, the mass percent of copper is 37wt%.
Silver-nickel electrical contact manufactured in the present embodiment to be tested, wherein the thickness of silver-nickel coating is 5 μm,
Wherein, in silver-nickel, silver-colored mass percentage is 18.31wt.%, and Sulfur tolerance test is carried out to silver-nickel electrical contact,
Corrosion resistance to sulfuric acid dew point result is 0.05056mg/cm2H, silver-nickel plating layer resistivity is in silver-nickel electrical contact
0.001 Ω m-0.002 Ω m, Sulfur tolerance test result are non-discolouring after immersing 30 minutes.
Claims (8)
1. a kind of method that electro-deposition prepares silver-nickel electrical contact, which is characterized in that comprise the following steps that：
Step 1, metallic matrix pre-treatment
Metallic matrix is polished, oil removing, acid etching, obtain pretreated metallic matrix；
Step 2, electroplate liquid is prepared
Choline chloride and ethylene glycol are mixed, heating stirring, until solution is in colourless transparent liquid, obtains choline chloride-second two
Alcohol eutectic solvent；Wherein, in molar ratio, choline chloride：Ethylene glycol=1：(1.5~3)；
Into choline chloride-ethylene glycol eutectic solvent, silver nitrate is added, it is completely molten to particles of silver nitrate to continue heating stirring
Solution, is then added nickel chloride, and continuous heating stirs to solution that be presented dark green transparent, obtains electroplate liquid；Wherein, by solid-to-liquid ratio
(unit g/L), silver nitrate：Choline chloride-ethylene glycol eutectic solvent=(30~80)：1, by solid-to-liquid ratio (unit g/L),
Nickel chloride：Choline chloride-ethylene glycol eutectic solvent=(20~40)：1；
Step 3, it is electroplated
Using above-mentioned electroplate liquid, DC electrodeposition is carried out to pretreated metallic matrix, obtains the silver-nickel on metallic matrix,
After cleaning, drying, as silver-nickel electrical contact；Wherein, in electrodeposition process, the temperature of electroplate liquid is 30~50 DEG C, and electric current is close
Degree is 1A/dm2~2A/dm2。
2. the method that electro-deposition as described in claim 1 prepares silver-nickel electrical contact, which is characterized in that the step 1
In, the metallic matrix, metal is one kind in carbon steel, low-alloy steel, copper, copper alloy, nickel or nickel alloy.
3. the method that electro-deposition as described in claim 1 prepares silver-nickel electrical contact, which is characterized in that the step 1
In, the polishing, specially：The sand paper that metallic matrix is used to different model respectively, according to sequential processes from thick to thin
Metal base surface obtains the smooth metallic matrix without apparent cut in surface.
4. the method that electro-deposition as described in claim 1 prepares silver-nickel electrical contact, which is characterized in that the step 1
In, the oil removing, specially：Metallic matrix after polishing is impregnated using alkaline mixed solution, soaking time 60
It~90 DEG C, after impregnating 10~30min, is rinsed with deionized water, obtains the metallic matrix after oil removing.
5. the method that electro-deposition as described in claim 1 prepares silver-nickel electrical contact, which is characterized in that the step 1
In, the acid etching, specially：Metallic matrix after oil removing is placed in the hydrochloric acid solution that molar concentration is 1~2mol/L
In, acid etching is carried out, 1~2min is handled at 40~50 DEG C, is rinsed with deionized water, obtains pretreated Metal Substrate
Body.
6. the method that electro-deposition as described in claim 1 prepares silver-nickel electrical contact, which is characterized in that the step 2
In, the heating stirring, heating temperature is 30~50 DEG C.
7. the method that electro-deposition as described in claim 1 prepares silver-nickel electrical contact, which is characterized in that the step 2
In, by solid-to-liquid ratio (unit g/L), silver nitrate：Choline chloride-ethylene glycol eutectic solvent=(34~51)：1.
8. the method that electro-deposition as described in claim 1 prepares silver-nickel electrical contact, which is characterized in that the step 3
In, electrode system used is two electrode systems.
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| CN109137015A (en) * | 2018-09-18 | 2019-01-04 | 惠州市碧欣环保科技有限公司 | A kind of environmental protection plating Ni-Ag-Ce2O3The preparation method of alloy layer |
| CN110681874A (en) * | 2019-11-07 | 2020-01-14 | 西南大学 | Preparation method and hydrogen evolution application of silver-nickel nanocluster |
| CN112663101A (en) * | 2019-10-15 | 2021-04-16 | 罗门哈斯电子材料有限责任公司 | Acidic aqueous silver-nickel alloy electroplating compositions and methods |
| CN114959818A (en) * | 2022-05-30 | 2022-08-30 | 阜阳师范大学 | Method for preparing super-hydrophobic coating by one-step electrodeposition in eutectic solvent |
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| CN109137015A (en) * | 2018-09-18 | 2019-01-04 | 惠州市碧欣环保科技有限公司 | A kind of environmental protection plating Ni-Ag-Ce2O3The preparation method of alloy layer |
| CN112663101A (en) * | 2019-10-15 | 2021-04-16 | 罗门哈斯电子材料有限责任公司 | Acidic aqueous silver-nickel alloy electroplating compositions and methods |
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| CN110681874B (en) * | 2019-11-07 | 2022-05-31 | 西南大学 | Preparation method and hydrogen evolution application of silver-nickel nanocluster |
| CN114959818A (en) * | 2022-05-30 | 2022-08-30 | 阜阳师范大学 | Method for preparing super-hydrophobic coating by one-step electrodeposition in eutectic solvent |
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