CN105401180A - Electroplating liquid of wear-resistant gold-plated film and electroplating method thereof - Google Patents
Electroplating liquid of wear-resistant gold-plated film and electroplating method thereof Download PDFInfo
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- CN105401180A CN105401180A CN201510976431.6A CN201510976431A CN105401180A CN 105401180 A CN105401180 A CN 105401180A CN 201510976431 A CN201510976431 A CN 201510976431A CN 105401180 A CN105401180 A CN 105401180A
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- electroplate liquid
- wear
- plated film
- gold
- working electrode
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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
- C25D3/48—Electroplating: Baths therefor from solutions of gold
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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
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
-
- 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
Abstract
The invention discloses electroplating liquid of a wear-resistant gold-plated film and an electroplating method thereof. The electroplating liquid comprises 5 to 100g/L of sulfite gold, 10 to 120g/L of 2-sulfo-5, 5-dimethyl hydantoin, 10 to 50g/L of succinimide, 40 to 100g/L of ethylene diamine tetra (methylene phosphonic acid) sodium, 10 to 40g/L of ethylenediamine tetramethylenephosphonic acid, 0.5 to 2g/L of thallium nitrate, 0.5 to 3g/L of SiC nano-particles, 0.5 to 2g/L of polyethylene glycol, 20 to 150g/L of sodium sulfite, and 2 to 10g/L of 1-(3-sulfopropyl)-isoquinoline betaine; the pH is 6.5 to 8. The electroplating liquid of the wear-resistant gold-plated film is environmentally friendly and stable; the SiC nanoparticles can greatly improve the wear resistance of the gold-plated film which is produced by electroplating with the electroplating liquid; the electroplating method is quick and stable, and the repeatability is high.
Description
Technical field
The present invention relates to a kind of technical field of electrogilding, be specifically related to a kind of electroplate liquid and electro-plating method thereof of wear-resisting gold-plated film.
Background technology
Gold utensil has very high stability, in plating piece plated surface one deck layer gold, not only has aesthetic property, also has the function of excellent protection against corrosion anti-discolouring, general in the application of souvenir badge (coin), jewellery and field of artware.But the wear resistance of Gold plated Layer is good not, and gold coated article surface easily produces cut.
Summary of the invention
Goal of the invention: for the deficiencies in the prior art, the invention provides a kind of electroplate liquid and electro-plating method thereof of wear-resisting gold-plated film, by adding the SiC nano particle of high-wearing feature to solve the problem of wear resistance in electroplate liquid.
Technical scheme: for achieving the above object, the present invention by the following technical solutions:
A kind of electroplate liquid of wear-resisting gold-plated film, comprise: sulfurous acid gold 5 ~ 100g/L, 2-sulfo--5, 5-T10 10 ~ 120g/L, succimide 10 ~ 50g/L, ethylene diamine tetra methylene phosphonic acid sodium 40 ~ 100g/L, ethylene diamine tetra methylene phosphonic acid 10 ~ 40g/L, thallium trinitrate (TTN) 0.5 ~ 2g/L, SiC nano particle 0.5 ~ 3g/L, polyoxyethylene glycol 0.5 ~ 2g/L, S-WAT 20 ~ 150g/L, 1-(3-sulfopropyl)-isoquinoline 99.9 trimethyl-glycine 2 ~ 10g/L, this electroplate liquid adopts ethylene diamine tetra methylene phosphonic acid to regulate pH at 6.5-8, and keep temperature of electroplating solution at 20 ~ 40 DEG C.This electroplate liquid with 2-sulfo--5,5-T10 be main coordination agent, succimide 10 ~ 50 is auxiliary coordination agent, effectively can improve the stability of electroplate liquid.
Further, the particle diameter of described SiC nano particle is 2 ~ 10nm.
Further, described SiC nano particle via polyethyleneimine-modified process, the SiC nano particle mobility crossed through polyethyleneimine-modified and favorable dispersity.
Based on an electro-plating method for the electroplate liquid of above-mentioned wear-resisting electrogilding film, comprise the following steps:
(1) pre-treatment: metal base is put into the acetone soln ultrasonic cleaning 2min that temperature is 45 ~ 55 DEG C, with after the ultrasonic 1min of dehydrated alcohol under room temperature, the hydrochloric acid putting into 1mol/L cleans 30s, and finally adopt deionized water rinsing 2 times, ultrapure water cleans 1 time;
(2) preplating: that step (1) is handled well puts into pre-plating solution, at 2A/dm
2current density under flash plate one deck layers of copper, first use washed with de-ionized water after taking-up, then clean with ultrapure water;
(3) electrogilding: the metal base after step (2) preplating is put into electroplate liquid, take platinized platinum as metal base after anode, preplating be working electrode, adopt square wave pulsed current method to carry out electrogilding, wherein, working electrode constantly swings and stirs.
Further, in described step (2), pre-plating solution comprises: cupric pyrophosphate 1 ~ 5g/L, methylsulphonic acid 5 ~ 50g/L, potassium pyrophosphate 5 ~ 20g/L, trolamine 10 ~ 20g/L, salt of wormwood 10 ~ 50g/L, nicotinic acid 0 ~ 50g/L, pH=6 ~ 7 of this pre-plating solution.
Further, in described step (3), square wave pulsed current method first applies a cathodic current ﹣ 0.1A/dm on the working electrode (s
2~ ﹣ 0.4A/dm
2, the burst length is 1000ms ~ 1500ms, then on this working electrode, applies an anodic current 0.4 ~ 1.2A/dm
2, the burst length is 1000ms ~ 1500ms, electroplates at 20 DEG C ~ 35 DEG C.
Further, the cycle index of square wave pulsed current method is 3 ~ 15 times in described step (3), and the thickness of Gold plated Layer increases gradually with the increase of cycle index.
Beneficial effect: compared with prior art, the electroplate liquid of a kind of wear-resisting gold-plated film provided by the invention, environmental protection is stablized, and the SiC nano particle wherein contained makes this electroplate liquid electroplate the gold-plated film wear resistance obtained greatly to improve, the electro-plating method fast and stable of this electroplate liquid, reproducible.
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
First electroplate liquid and pre-plating solution is prepared, electroplate liquid comprises the component of following mass body volume concentrations: sulfurous acid gold 5g/L, 2-sulfo--5, 5-T10 10g/L, succimide 10g/L, ethylene diamine tetra methylene phosphonic acid sodium 40g/L, ethylene diamine tetra methylene phosphonic acid 10g/L, thallium trinitrate (TTN) 0.5g/L, SiC nano particle 0.5g/L, polyoxyethylene glycol 0.5g/L, S-WAT 20g/L, 1-(3-sulfopropyl)-isoquinoline 99.9 trimethyl-glycine 2g/L, this cyanideless electro-plating liquid adopts ethylene diamine tetra methylene phosphonic acid to regulate pH 7.3, and keep cyanideless electro-plating liquid temp at 25 DEG C, wherein SiC nano grain surface is via polyethyleneimine-modified process, its particle diameter is 3nm.
Pre-plating solution comprises cupric pyrophosphate 1g/L, methylsulphonic acid 5g/L, potassium pyrophosphate 5g/L, trolamine 10g/L, salt of wormwood 10g/L, the pH=6 of this pre-plating solution.
Nickel sheet is put into the acetone soln ultrasonic cleaning 2min that temperature is 45 DEG C, with after the ultrasonic 1min of dehydrated alcohol under room temperature, the hydrochloric acid putting into 1mol/L cleans 30s, and finally adopt deionized water rinsing 2 times, ultrapure water cleans 1 time; Copper sheet after having cleaned is placed in pre-plating solution, at 2A/dm
2current density under flash plate one deck layers of copper, first use washed with de-ionized water after taking-up, then clean with ultrapure water.
Nickel sheet after preplating puts into electroplate liquid, is that the metal base after anode, preplating is working electrode with platinized platinum, adopts square wave pulsed current method to carry out electrogilding, first applies a cathodic current ﹣ 0.1A/dm on the working electrode (s
2, the burst length is 1000ms, then on this working electrode, applies an anodic current 0.4A/dm
2, the burst length is 1000ms, carries out circulation plating 3 times at 20 DEG C.Wherein, working electrode constantly swings and stirs, the Gold plated Layer golden bright obtained and excellent in abrasion resistance.
Embodiment 2
First electroplate liquid and pre-plating solution is prepared.Electroplate liquid comprises the component of following mass body volume concentrations: sulfurous acid gold 50g/L, 2-sulfo--5, 5-T10 60g/L, succimide 30g/L, ethylene diamine tetra methylene phosphonic acid sodium 70g/L, ethylene diamine tetra methylene phosphonic acid 25g/L, thallium trinitrate (TTN) 1g/L, SiC nano particle 2g/L, polyoxyethylene glycol 1g/L, S-WAT 80g/L, 1-(3-sulfopropyl)-isoquinoline 99.9 trimethyl-glycine 6g/L, this cyanideless electro-plating liquid adopts ethylene diamine tetra methylene phosphonic acid to regulate pH 8, and keep cyanideless electro-plating liquid temp at 35 DEG C, wherein SiC nano grain surface is via polyethyleneimine-modified process, its particle diameter is 5nm.Pre-plating solution comprises cupric pyrophosphate 3g/L, methylsulphonic acid 15g/L, potassium pyrophosphate 12.5g/L, trolamine 15g/L, salt of wormwood 32g/L, nicotinic acid 27g/L, the pH=6.3 of this pre-plating solution.
Nickel sheet is put into the acetone soln ultrasonic cleaning 2min that temperature is 55 DEG C, with after the ultrasonic 1min of dehydrated alcohol under room temperature, the hydrochloric acid putting into 1mol/L cleans 30s, and finally adopt deionized water rinsing 2 times, ultrapure water cleans 1 time; Copper sheet after having cleaned is placed in pre-plating solution, at 2A/dm
2current density under flash plate one deck layers of copper, first use washed with de-ionized water after taking-up, then clean with ultrapure water.
Nickel sheet after preplating puts into electroplate liquid, is that the metal base after anode, preplating is working electrode with platinized platinum, adopts square wave pulsed current method to carry out electrogilding, first applies a cathodic current ﹣ 0.22A/dm on the working electrode (s
2, the burst length is 1500ms, then on this working electrode, applies an anodic current 0.82A/dm
2, the burst length is 1500ms, carries out circulation plating 10 times at 35 DEG C.Wherein, working electrode constantly swings and stirs, the Gold plated Layer golden bright obtained and excellent in abrasion resistance.
Embodiment 3
First electroplate liquid and pre-plating solution is prepared.Electroplate liquid comprises the component of following mass body volume concentrations: sulfurous acid gold 70g/L, 2-sulfo--5,5-T10 96g/L, succimide 37g/L, ethylene diamine tetra methylene phosphonic acid sodium 69g/L, ethylene diamine tetra methylene phosphonic acid 25g/L, thallium trinitrate (TTN) 2g/L, SiC nano particle 2g/L, polyoxyethylene glycol 2g/L, S-WAT 73g/L, 1-(3-sulfopropyl)-isoquinoline 99.9 trimethyl-glycine 9g/L, this electroplate liquid adopts ethylene diamine tetra methylene phosphonic acid to regulate pH 8, wherein SiC nano grain surface is via polyethyleneimine-modified process, and its particle diameter is 10nm.Pre-plating solution comprises cupric pyrophosphate 5g/L, methylsulphonic acid 50g/L, potassium pyrophosphate 20g/L, trolamine 20g/L, salt of wormwood 50g/L, nicotinic acid 50g/L, the pH=6.1 of this pre-plating solution.
Nickel sheet is put into the acetone soln ultrasonic cleaning 2min that temperature is 55 DEG C, with after the ultrasonic 1min of dehydrated alcohol under room temperature, the hydrochloric acid putting into 1mol/L cleans 30s, and finally adopt deionized water rinsing 2 times, ultrapure water cleans 1 time; Copper sheet after having cleaned is placed in pre-plating solution, at 2A/dm
2current density under flash plate one deck layers of copper, first use washed with de-ionized water after taking-up, then clean with ultrapure water.
Nickel sheet after preplating puts into electroplate liquid, is that the metal base after anode, preplating is working electrode with platinized platinum, adopts square wave pulsed current method to carry out electrogilding, first applies a cathodic current ﹣ 0.22A/dm on the working electrode (s
2, the burst length is 1500ms, then on this working electrode, applies an anodic current 0.82A/dm
2, the burst length is 1500ms, carries out circulation plating 10 times at 35 DEG C.Wherein, working electrode constantly swings and stirs, the Gold plated Layer golden bright obtained and excellent in abrasion resistance.
Nickel sheet is put into the acetone soln ultrasonic cleaning 2min that temperature is 55 DEG C, with after the ultrasonic 1min of dehydrated alcohol under room temperature, the hydrochloric acid putting into 1mol/L cleans 30s, and finally adopt deionized water rinsing 2 times, ultrapure water cleans 1 time; Copper sheet after having cleaned is placed in pre-plating solution, at 2A/dm
2current density under flash plate one deck layers of copper, first use washed with de-ionized water after taking-up, then clean with ultrapure water.
Nickel sheet after preplating puts into electroplate liquid, is that the metal base after anode, preplating is working electrode with platinized platinum, adopts square wave pulsed current method to carry out electrogilding, first applies a cathodic current ﹣ 0.4A/dm on the working electrode (s
2, the burst length is 1500ms, then on this working electrode, applies an anodic current 1.2A/dm
2, the burst length is 1500ms, carries out circulation plating 15 times at 35 DEG C.Wherein, working electrode constantly swings and stirs, the Gold plated Layer golden bright obtained and excellent in abrasion resistance.
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 (7)
1. the electroplate liquid of a wear-resisting gold-plated film, it is characterized in that: described electroplate liquid comprises: sulfurous acid gold 5 ~ 100g/L, 2-sulfo--5, 5-T10 10 ~ 120g/L, succimide 10 ~ 50g/L, ethylene diamine tetra methylene phosphonic acid sodium 40 ~ 100g/L, ethylene diamine tetra methylene phosphonic acid 10 ~ 40g/L, thallium trinitrate (TTN) 0.5 ~ 2g/L, SiC nano particle 0.5 ~ 3g/L, polyoxyethylene glycol 0.5 ~ 2g/L, S-WAT 20 ~ 150g/L, 1-(3-sulfopropyl)-isoquinoline 99.9 trimethyl-glycine 2 ~ 10g/L, this electroplate liquid adopts ethylene diamine tetra methylene phosphonic acid to regulate pH at 6.5-8, and keep temperature of electroplating solution at 20 ~ 40 DEG C.
2. the electroplate liquid of wear-resisting gold-plated film according to claim 1, is characterized in that: the particle diameter of described SiC nano particle is 2 ~ 10nm.
3. the electroplate liquid of wear-resisting gold-plated film according to claim 1, is characterized in that: described SiC nano particle is via polyethyleneimine-modified process.
4., based on an electro-plating method for the electroplate liquid of the wear-resisting gold-plated film described in any one of claim 1-3, it is characterized in that: comprise the following steps:
(1) pre-treatment: metal base is put into the acetone soln ultrasonic cleaning 2min that temperature is 45 ~ 55 DEG C, with after the ultrasonic 1min of dehydrated alcohol under room temperature, the hydrochloric acid putting into 1mol/L cleans 30s, and finally adopt deionized water rinsing 2 times, ultrapure water cleans 1 time;
(2) preplating: that step (1) is handled well puts into pre-plating solution, at 2A/dm
2current density under flash plate one deck layers of copper;
(3) electrogilding: the metal base after step (2) preplating is put into electroplate liquid, take platinized platinum as metal base after anode, preplating be working electrode, adopt square wave pulsed current method to carry out electrogilding, wherein, working electrode constantly swings and stirs.
5. the electro-plating method of the electroplate liquid of wear-resisting gold-plated film according to claim 4, it is characterized in that: in described step (2), pre-plating solution comprises: cupric pyrophosphate 1 ~ 5g/L, methylsulphonic acid 5 ~ 50g/L, potassium pyrophosphate 5 ~ 20g/L, trolamine 10 ~ 20g/L, salt of wormwood 10 ~ 50g/L, nicotinic acid 0 ~ 50g/L, pH=6 ~ 7 of this pre-plating solution.
6. the electro-plating method of the electroplate liquid of wear-resisting gold-plated film according to claim 4, is characterized in that: in described step (3), square wave pulsed current method first applies a cathodic current ﹣ 0.1A/dm on the working electrode (s
2~ ﹣ 0.4A/dm
2, the burst length is 1000ms ~ 1500ms, then on this working electrode, applies an anodic current 0.4 ~ 1.2A/dm
2, the burst length is 1000ms ~ 1500ms, electroplates at 20 DEG C ~ 35 DEG C.
7. the electro-plating method of the electroplate liquid of wear-resisting gold-plated film according to claim 4, is characterized in that: in described step (3), the cycle index of square wave pulsed current method is 3 ~ 15 times.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107385486A (en) * | 2016-05-16 | 2017-11-24 | 中国科学院微电子研究所 | The method of pulse plating gold and the gold plate of formation |
| JP2021181600A (en) * | 2020-05-19 | 2021-11-25 | 日本エレクトロプレイテイング・エンジニヤース株式会社 | Electrolytic gold alloy plating bath and electrolytic gold alloy plating method |
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