CN105463535A - Electroplating method of cyanide-free copper-zinc electroplating solution containing ionic liquid - Google Patents
Electroplating method of cyanide-free copper-zinc electroplating solution containing ionic liquid Download PDFInfo
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- CN105463535A CN105463535A CN201510976246.7A CN201510976246A CN105463535A CN 105463535 A CN105463535 A CN 105463535A CN 201510976246 A CN201510976246 A CN 201510976246A CN 105463535 A CN105463535 A CN 105463535A
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- Prior art keywords
- ionic liquid
- electroplate liquid
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- copper zinc
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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
- C25D3/66—Electroplating: Baths therefor from melts
- C25D3/665—Electroplating: Baths therefor from melts from ionic liquids
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/021—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material including at least one metal alloy layer
-
- 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
- C25D5/18—Electroplating using modulated, pulsed or reversing current
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Mechanical Engineering (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The invention discloses an electroplating method of a cyanide-free copper-zinc electroplating solution containing an ionic liquid. The electroplating method comprises the following steps: (1) preparation of the cyanide-free copper-zinc electroplating solution; (2) pretreatment of a stainless steel workpiece; (3) copper pre-plating; (4) copper-zinc alloy electroplating; and (5) after-treatment. The electroplating method provided by the present invention solves the problem of poor solubility between metal ions and the ionic liquid; the electroplating solution contains the ionic liquid additive and thus is non-toxic and pollution-free, and low in energy consumption; meanwhile, due to a relatively low quantity of the added ionic liquid, no production cost is increased; the electroplating method can be used within a relatively wide current density range; and a coating obtained through electroplating under a continuously increased current density is golden yellow, continuous and even, and compact, and further good in binding force with a substrate, and resistant to high temperatures and abrasion.
Description
Technical field
The present invention relates to field of electroplating, be specifically related to a kind of electro-plating method without cyanogen copper zinc electroplate liquid containing ionic liquid for coinage.
Background technology
Golden plating is widely used in decorative electroplating.But proof gold plating because the price of gold is expensive, hardness is low, wear no resistance, make it apply and be restricted.The flavous color and luster of imitation gold deposit can meet ornamental requirement, hardness, the wear resistance of coating improve greatly, it is with low cost, be used for the decorative electroplating on the parts such as jewellery, handicraft, light fixture, button, wrist-watch, lighter, there is obvious economic benefit and vast potential for future development.Imitative gold (copper zinc alloy) plating uses prussiate plating, and coating crystallization is careful, solution dispersibility and covering power good, tint is similar to proof gold, but this technique uses the prussiate of severe toxicity, huge to the harm of human body and environment.
In recent years, be developed multiple Cyanida free imitative electrogilding solution, as pyrophosphate salt system, tartrate system, HEDP system, citric acid systems etc.These electroplate liquids respectively have advantage, but also there is own limitations, cannot fundamentally substitute imitation gold plating liquid.
The title that ionic liquid have " green solvent ", it is a kind of organic liquid be made up of negative and positive two kinds of ions, is also referred to as the fused salt under low temperature.Ionic liquid does not have a lot of good characteristic as solvent, and such as its vapour pressure is approximately zero, volatile and do not produce pollution problem, has good ionic conductivity and thermal conductivity, also possesses high thermal stability and high heat capacity simultaneously.Start in recent years to be applied to metal electrodeposition and achieve preliminary study progress.Ionic liquid is poorly soluble to common metal salt, affects deposition layer quality afterwards.Therefore, the application of ionic liquid in metal electrodeposition needs further development and exploration.
Summary of the invention
Goal of the invention: for the deficiencies in the prior art, the invention provides a kind of for coinage containing the electro-plating method without cyanogen copper zinc electroplate liquid of ionic liquid, make method simply, electroplate the coating that obtains and basal body binding force is good, uniform color is bright, method is reproducible.
Technical scheme: for achieving the above object, the present invention by the following technical solutions:
Containing the electro-plating method without cyanogen copper zinc electroplate liquid of ionic liquid, comprise the following steps:
(1) prepare without cyanogen copper zinc electroplate liquid, electroplate liquid comprises the component of following quality volume fraction: potassium pyrophosphate 150 ~ 200g/L, anhydrous cupric sulfate 48 ~ 96g/L, zinc sulfate 5 ~ 15g/L, glycerol 10 ~ 30g/L, succimide 10 ~ 30g/L, nitrilotriacetic acid(NTA) 20 ~ 30g/L, tetra-sodium 70 ~ 100g/L, benzotriazole 6-10g/L and ion liquid addictive 30 ~ 100mg/L, wherein said ion liquid addictive is 1-ethyl-3-methylimidazole diethyl phosphoric acid salt, 1-ethyl-3-methylimidazole dimethyl phosphate salt, 1, 3-diethyl imidazolium diethyl phosphoric acid salt or 1, one or more in 3-diethyl imidazolium dimethyl phosphate salt, ammoniacal liquor regulates pH to 8.0-10.5,
(2) stainless steel work-piece pre-treatment, by oil removing after the polishing of stainless steel work-piece surface finish, then carry out acidic activated and in and clean;
(3) copper pre-plating, preplating one deck layers of copper on the stainless steel work-piece after pre-treatment, the thickness of described layers of copper is 200-800nm;
(4) copper zinc alloy plating, is placed in electroplate liquid using the stainless steel work-piece after copper pre-plating as negative electrode, and using inertia pole plate as anode, the temperature keeping electroplate liquid is 20-50 DEG C, passes into electric current and electroplates.
(5) aftertreatment, is placed in washed with de-ionized water by the stainless steel work-piece through plating, then places in High Temperature Furnaces Heating Apparatus and heat-treats, packaging after cooling.
Further, in described step (2), oil removing is alkaline degreasing or ultrasonic oil removing.
Further, the condition of described ultrasonic oil removing is: immersed by the workpiece after polishing in the mixing solutions of acetone and methylene dichloride 1:1 (v:v), ultrasonic cleaning 1 minute, for removing the organism on surface, adopt dehydrated alcohol ultrasonic cleaning 2min afterwards, use deionized water rinsing again 2 times, finally use ultrapure water 1 time.
Further, in described step (3), the method for copper pre-plating is the one in sputtering method, vapour deposition method or electroless plating method.
Further, in described step (4), inertia pole plate is platinized platinum or graphite.
Further, the distance in described step (4) between negative electrode and anode is 16-30cm.
Further, in described step (4), electric current is that current density increases.
Further, in described step (4), electric current is that current density linearly increases.
Further, the middle electric current of described step (4) is with per minute 0.1-0.2A/dm
2speed from 0A/dm
2linearly be increased to 4-6A/dm
2, galvanostatic deposition 20-30min subsequently.
Further, described step (4) adopts magnetic stirring apparatus to stir while plating.
In step (5), heat treated condition is under reducing atmosphere, and 550-600 DEG C of heating 50-70min, reducing atmosphere uses H
2or H
2-Ar.
Beneficial effect: compared with prior art, electro-plating method provided by the invention has the following advantages:
(1) solve problem poorly soluble between metal ion and ionic liquid, can use in water solution system, the electroplate liquid system dispersiveness of preparation and good stability; Electroplate liquid of the present invention contains ion liquid addictive, makes electroplate liquid nontoxic pollution-free, energy consumption low, and addition is less simultaneously, does not increase production cost.
(2) electro-plating method of the present invention can use in wider current density range, and electroplates under the current density increased continuously, the coating color obtained is golden yellow, continuous uniform, densification, good with basal body binding force, heat resistant and wear resistant.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described, and the description of specific embodiment is only example in essence, instead of intend to limit content disclosed by the invention and application thereof or use.
Embodiment 1
Preparation electroplate liquid, comprise the component of following mass body volume concentrations: potassium pyrophosphate 200g/L, anhydrous cupric sulfate 92g/L, zinc sulfate 13g/L, glycerol 29g/L, succimide 28g/L, nitrilotriacetic acid(NTA) 26g/L, tetra-sodium 100g/L, benzotriazole 10g/L and 1-ethyl-3-methylimidazole diethyl phosphoric acid salt 95mg/L, use ammoniacal liquor to regulate pH to 9.7.
Using stainless steel work-piece through sanding and polishing, alkaline degreasing, acidic activated, neutralization cleaning after as negative electrode, the stainless steel work-piece after pre-treatment will use sputtering method preplating one deck 200nm layers of copper.Insert subsequently fill above-mentioned electroplate liquid Hull Cell in, be anode with platinized platinum, the distance between negative electrode and anode is 16cm, electroplates under magnetic stirring with the rotating speed of 200r/min, and the electric current of plating is with per minute 0.1A/dm
2speed from 0A/dm
2linearly be increased to 4A/dm
2, galvanostatic deposition 20min, obtains coating subsequently, uses the electroplate liquid that washed with de-ionized water coating surface is remaining, is then placed on logical H in High Temperature Furnaces Heating Apparatus
2heat-treat at 600 DEG C of heating 50min, packaging after cooling.
This coating adopts GB/T13913-92 detect with the bonding force of base material and toast 5min at 300 DEG C, and without bubbling, arch skin situation occurs, illustrate that between this coating matrix, bonding force and high thermal resistance are good, smooth at metallography microscope Microscopic observation light, color is golden yellow.
Embodiment 2
Electroplate liquid composition and embodiment 1 basic simlarity, difference is that embodiment 2 intermediate ion liquid is 1-ethyl-3-methylimidazole dimethyl phosphate salt 84.9mg/L.
Stainless steel work-piece pre-treatment, first cleans in the alkaline cleaning fluid of 50 DEG C, afterwards at room temperature pickling 3min, finally use deionized water and ultrapure water rinsing.Stainless steel work-piece after pre-treatment will use vapour deposition method preplating one deck 600nm layers of copper.Being inserted by stainless steel work-piece after pre-treatment in the Hull Cell filling above-mentioned electroplate liquid subsequently, take platinized platinum as anode, and the distance between negative electrode and anode is 20cm, electroplates under magnetic stirring with the rotating speed of 200r/min, and the electric current of plating is with per minute 0.2A/dm
2speed from 0A/dm
2linearly be increased to 5A/dm
2, galvanostatic deposition 26min, obtains coating subsequently, uses the electroplate liquid that washed with de-ionized water coating surface is remaining, is then placed on logical H in High Temperature Furnaces Heating Apparatus
2+ Ar heat-treats at 550 DEG C of heating 60min, packaging after cooling.
This coating adopts GB/T13913-92 detect with the bonding force of base material and toast 5min at 300 DEG C, and without bubbling, arch skin situation occurs, illustrate that between this coating and matrix, bonding force and high thermal resistance are good, smooth at metallography microscope Microscopic observation light, color is golden yellow.
Embodiment 3
Electroplate liquid comprises the component of following mass body volume concentrations: potassium pyrophosphate 160g/L, anhydrous cupric sulfate 72g/L, zinc sulfate 10g/L, glycerol 20g/L, succimide 20g/L, nitrilotriacetic acid(NTA) 23g/L, tetra-sodium 100g/L, benzotriazole 8g/L and 1,3-diethyl imidazolium dimethyl phosphate salt 52mg/L, use ammoniacal liquor to regulate pH to 9.1, the temperature of electroplate liquid controls at 20-40 DEG C.
Stainless steel work-piece pre-treatment, first cleans in the alkaline cleaning fluid of 50 DEG C, afterwards at room temperature pickling 2min, finally use deionized water and ultrapure water rinsing.Stainless steel work-piece after pre-treatment will use vapour deposition method preplating one deck 760nm layers of copper.Stainless steel work-piece after copper pre-plating is placed in above-mentioned electroplate liquid as negative electrode, graphite is anode, and the temperature keeping electroplate liquid is 25 DEG C, and the distance between negative electrode and anode is 30cm, electroplate under magnetic stirring with the rotating speed of 200r/min, the electric current of plating is with per minute 0.2A/dm
2speed from 0A/dm
2linearly be increased to 6A/dm
2, galvanostatic deposition 30min, obtains coating subsequently, uses the electroplate liquid that washed with de-ionized water coating surface is remaining, is then placed on logical H in High Temperature Furnaces Heating Apparatus
2+ Ar heat-treats at 550 DEG C of heating 60min, packaging after cooling.
This coating adopts GB/T13913-92 detect with the bonding force of base material and toast 5min at 300 DEG C, and without bubbling, arch skin situation occurs, illustrate that between this coating and matrix, bonding force and high thermal resistance are good, smooth at metallography microscope Microscopic observation light, color is golden yellow.
Embodiment 4
Embodiment and embodiment 3 basic simlarity, difference is, embodiment 4 intermediate ion liquid is 1,3-diethyl imidazolium diethyl phosphoric acid salt 65.5mg/L.
Electroplate liquid is recycling repeatedly and is reusing after placing 1 month, and the coating performance obtained does not decline, and this electroplate liquid good stability is described.
Above embodiment just plays illustrated example effect to technical conceive of the present invention; can not limit the scope of the invention with this; those skilled in the art are not departing from the spirit and scope of technical solution of the present invention; modify and be equal to replacement, all should drop within protection scope of the present invention.
Claims (10)
1., containing the electro-plating method without cyanogen copper zinc electroplate liquid of ionic liquid, it is characterized in that, comprise the following steps:
(1) prepare without cyanogen copper zinc electroplate liquid, electroplate liquid comprises the component of following quality volume fraction: potassium pyrophosphate 150 ~ 200g/L, anhydrous cupric sulfate 48 ~ 96g/L, zinc sulfate 5 ~ 15g/L, glycerol 10 ~ 30g/L, succimide 10 ~ 30g/L, nitrilotriacetic acid(NTA) 20 ~ 30g/L, tetra-sodium 70 ~ 100g/L, benzotriazole 6-10g/L and ion liquid addictive 30 ~ 100mg/L, wherein said ion liquid addictive is 1-ethyl-3-methylimidazole diethyl phosphoric acid salt, 1-ethyl-3-methylimidazole dimethyl phosphate salt, 1, 3-diethyl imidazolium diethyl phosphoric acid salt or 1, one or more in 3-diethyl imidazolium dimethyl phosphate salt, ammoniacal liquor regulates pH to 8.0-10.5,
(2) stainless steel work-piece pre-treatment, by oil removing after the polishing of stainless steel work-piece surface finish, then carry out acidic activated and in and clean;
(3) copper pre-plating, preplating one deck layers of copper on the stainless steel work-piece after pre-treatment, the thickness of described layers of copper is 200-800nm;
(4) copper zinc alloy plating, is placed in electroplate liquid using the stainless steel work-piece after copper pre-plating as negative electrode, and using inertia pole plate as anode, the temperature keeping electroplate liquid is 20-50 DEG C, passes into electric current and electroplates;
(5) aftertreatment, is placed in washed with de-ionized water by the stainless steel work-piece through plating, then places in High Temperature Furnaces Heating Apparatus and heat-treats, packaging after cooling.
2. the electro-plating method without cyanogen copper zinc electroplate liquid containing ionic liquid according to claim 1, is characterized in that, in described step (2), oil removing is alkaline degreasing or ultrasonic oil removing.
3. the electro-plating method without cyanogen copper zinc electroplate liquid containing ionic liquid according to claim 2, it is characterized in that, the condition of described ultrasonic oil removing is: immersed by the workpiece after polishing in the mixing solutions of acetone and methylene dichloride 1:1 (v:v), ultrasonic cleaning 1 minute, for removing the organism on surface, adopt dehydrated alcohol ultrasonic cleaning 2min afterwards, then use deionized water rinsing 2 times, finally use ultrapure water 1 time.
4. the electro-plating method without cyanogen copper zinc electroplate liquid containing ionic liquid according to claim 1, is characterized in that, in described step (3), the method for copper pre-plating is the one in sputtering method, vapour deposition method or electroless plating method.
5. the electro-plating method without cyanogen copper zinc electroplate liquid containing ionic liquid according to claim 1, is characterized in that, in described step (4), inertia pole plate is platinized platinum or graphite.
6. the electro-plating method without cyanogen copper zinc electroplate liquid containing ionic liquid according to claim 1, is characterized in that, the distance in described step (4) between negative electrode and anode is 16-30cm.
7. the electro-plating method without cyanogen copper zinc electroplate liquid containing ionic liquid according to claim 1, is characterized in that, in described step (4), electric current is that current density increases.
8. the electro-plating method without cyanogen copper zinc electroplate liquid containing ionic liquid according to claim 7, is characterized in that, in described step (4), electric current is that current density linearly increases.
9. the electro-plating method without cyanogen copper zinc electroplate liquid containing ionic liquid according to claim 7, is characterized in that, in described step (4), electric current is with per minute 0.1-0.2A/dm
2speed from 0A/dm
2linearly be increased to 4-6A/dm
2, galvanostatic deposition 20-30min subsequently.
10. the electro-plating method without cyanogen copper zinc electroplate liquid containing ionic liquid according to claim 1, is characterized in that, described step (4) adopts magnetic stirring apparatus to stir while plating.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510976246.7A CN105463535A (en) | 2015-12-23 | 2015-12-23 | Electroplating method of cyanide-free copper-zinc electroplating solution containing ionic liquid |
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| CN201510976246.7A CN105463535A (en) | 2015-12-23 | 2015-12-23 | Electroplating method of cyanide-free copper-zinc electroplating solution containing ionic liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114457394A (en) * | 2022-01-17 | 2022-05-10 | 成都飞机工业（集团）有限责任公司 | Electrolyte and preparation method and application thereof |
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Application publication date: 20160406 |