CN101629313A - Double-pulse plating silver solution and technique thereof - Google Patents

Double-pulse plating silver solution and technique thereof Download PDF

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Publication number
CN101629313A
CN101629313A CN200910060261A CN200910060261A CN101629313A CN 101629313 A CN101629313 A CN 101629313A CN 200910060261 A CN200910060261 A CN 200910060261A CN 200910060261 A CN200910060261 A CN 200910060261A CN 101629313 A CN101629313 A CN 101629313A
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silver
pulse
plating
solution
double
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高升文
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No 5719 Factory of PLA
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No 5719 Factory of PLA
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Abstract

The invention discloses a double-pulse plating silver solution and a technique thereof, which has the advantages of high plating speed, high coating hardness, good abrasion performance and strong anti-tarnishing capacity. The plating solution has no organic additive with good maintainability and stability, increases the content of potassium cyanide, a certain amount of potassium nitrate is added in the plating solution, thus improving conductivity of the plating silver solution, increasing the concentration of silver ions, ensuring that enough silver ions can be deposited on the cathode surface at the moment of pulse, and being favor of improving deposition speed of silver coatings. The content control of each component of the solution is allowed to be changed in a larger range, especially the content change of the free cyanide needs no strict limitation. The grain of the silver coating is refined with small seepage hydrogen amount and impurity absorption, and the silver coating has high fineness and low internal stress.

Description

A kind of double-pulse plating silver solution and technology thereof
Technical field
The present invention relates to a kind of double-pulse plating silver solution and technology thereof.
Background technology
Pulse plating is a kind of electroplating technology that grows up the sixties in 20th century, uses on the high speed electrodeposition of various conventional platings, and practice and experiment show that all pulse plating all has preferable performance, so the pulse plating development is very fast.
The principle of work of pulse plating mainly is to utilize the tension and relaxation of electric current (or voltage) pulse to increase the activation polarization of negative electrode and the concentration polarization of reduction negative electrode.When current lead-through, be deposited fully near the metal ion of negative electrode; When electric current turn-offed, the discharge ion around the negative electrode returned to starting point concentration.The continuous repetition pulse electric current in cycle is mainly used in reduction of metal ion like this, thereby improves the physical and chemical performance of coating.The pulse plating parameter mainly contains: pulse current density i p, average current density i m, turn-off time t Off, ON time t On, recurrence interval T (or pulse-repetition f=1/T), work than (dutycycle) D=t On/ (t On+ t Off).
0.3,0.4,0.5A/dm patent CN101008095 discloses a kind of pulse silver-coating method, and frequency is 800HZ, break make ratio r%:8,16,24, current density: 2, solution composition: silver chloride 30-40 grams per liter, potassium cyanide 45-80 grams per liter, salt of wormwood 18-50 grams per liter, dithiocarbonic anhydride 0.04 grams per liter, (28%) 0.8 milliliter/liter in ammonium hydroxide, free potassuim cyanide 30-55 grams per liter, gained coating is smoothly careful, and bonding force and anti-sulphur are good.
" application is covered with paint, lacquer, colour wash, etc. and electroplated " 2006.4 (5) .30-34 disclose a kind of pulse silver-coating parameter: frequency is 800HZ, work ratio 20%, average current density: 0.8-1A/dm 2, negative-going pulse: frequency is 800HZ, work ratio 10%, average current density: 0.05-0.1A/dm 2, solution composition: Silver Nitrate 31-47 grams per liter (or silver chloride 26-46 grams per liter), total potassium cyanide 45-80 grams per liter, salt of wormwood 18-50 grams per liter, potassium cyanide 10-56 grams per liter, the crystallization of gained coating is careful, bonding force and voidage are good, and microhardness and wear resistance obviously are better than direct current coating.
" material protection " 2005.38 (7) .21-24 disclose a kind of bidirectional pulse non-cyanide silver coating technology, gained coating minute surface light, and discoloration-resisting and wet fastness significantly improve.
" electroplate and cover with paint, lacquer, colour wash, etc. " 2005.24 (2) .42-43 disclose a kind of DMS two pulse cyaniding plant of silver Technology, add brightening agent, the silvered film of the light of class, and discoloration-resisting improves, and can save silver 20% every year.
Summary of the invention:
The purpose of this invention is to provide a kind of double-pulse plating silver solution and technology thereof, hardness height, the wear resistance of electroplating velocity height, coating is good, anti-tarnishing ability is strong, and plating bath does not contain organic additive, maintainability and good stability.Double-pulse plating is to adopt forward and negative-going pulse electric current to carry out electric plating method.
The invention provides a kind of double-pulse plating silver solution composition is:
Saltpetre KNO 360g/L～100g/L
Silver chloride AgCl 70g/L～80g/L
Potassium cyanide KCN (always) 180g/L～190g/L
Potassium cyanide KCN (dissociating) 110g/L～120g/L
Solvent is a water
The silver plated processing parameter of two pulse is:
Temperature: room temperature
Mean Forward Current density i + m: 0.5A/dm 2～1.5A/dm 2
Negative sense average current density i - m: 0.25A/dm 2～0.5A/dm 2
Forward conduction time t + On: 0.2ms～0.4ms
Negative sense ON time t - On: 0.1ms～0.2ms
The forward period T +: 0.8ms～1.5ms
The negative sense period T -: 0.8ms～1.5ms
Positive negative pulse stuffing wave number ratio is 4: 1--8: 1 or 32: 4-32: 8
Direct impulse work ratio: 0.1～0.25
Negative-going pulse work ratio: 0.05～0.2
In the two pulse silver plating solution, the scope of selectable current density is very wide, and average current density is 0.5-1.5A/dm 2, all can obtain careful coating.
The direct impulse cycle equals negative-going pulse cycle (T +=T -), the recurrence interval can obtain test effect preferably in the 0.5ms-1.5ms scope, and the undue chopped pulse cycle is not useful.Electrode/electro is separated the existing electrostatic double layer of solution interface, the capacity effect that under pulse condition, is produced, directly affect the selection of recurrence interval, have only pulse width to be far longer than electrostatic double layer duration of charging, inter-train pause time and be far longer than electrostatic double layer discharge time, could guarantee output ideal square wave, use the too short recurrence interval to be difficult to realize above-mentioned two conditions;
Direct impulse work ratio is in 0.1～0.25 scope, and silver layer sedimentation velocity, degree of grain refinement, microhardness, wear resistance are better; Direct impulse work comparison coating deposition plays leading role, along with direct impulse work ratio reduces, helps obtaining the careful coating of crystallization, but also correspondingly slows down sedimentation velocity.Negative-going pulse work is than generally being set at 0.05～0.2.The selection of negative-going pulse work ratio is opposite with the selection of direct impulse work ratio, and negative-going pulse work ratio is big more, and crystal grain is thin more, and when negative-going pulse work ratio was too low, negative-going pulse was ineffective, and when other parameter constants, the test piece edge is obviously coarse; Because the existence of negative-going pulse can make grain refining, reduce the absorption of amount of hydrogen infiltration and impurity, reduce the silvering internal stress, excessive negative-going pulse electric current also can cause anode passivation;
The positive negative pulse stuffing wave number is than at 4: 1 between 8: 1 the time, and the coating effect is better.Reduce positive negative pulse stuffing wave number ratio, can directly influence coating deposition rate.When the wave number ratio is reduced to 1: 1, because electrostatic double layer replaces charging and discharging, consumed portion of energy, weakened the effect of pulse plating.
When the direct impulse ON time was 0.2-0.4ms, the coating crystallization was careful, and ON time is too short, was unfavorable for the formation of square wave, formed pulse direct current easily; ON time is long, and coating is coarse.When the negative-going pulse ON time was 0.1-0.2ms, the coating crystallization was careful, and ON time is too short, did not have the effect of reverse impulse; ON time is long, influences coating deposition rate.
The electrosilvering technology of double-pulse plating silver solution mainly comprises the steps:
A copper and copper alloy two pulse silver plating process flow process: weak etch, 5 pre-etch, 3 1) electrochemical degreasing, 2)) bright pickling, 4)) neutralization, 6) pre-copper facing, 7) two pulse silver-plated, 8) dehydration, 9) dry, 10) thermal treatment;
B stainless steel two pulse silver plating process flow process: weak etch, 4 pickling, 3 1) electrochemical degreasing, 2))) nickel preplating, 5) prepulsing silver-plated, 6) pulse silver-coating, 7) dry, 8) thermal treatment.
The present invention has following beneficial effect than prior art:
1) the two pulse silver plating solution is not added with organic additive, safeguards easily;
2) increase potassium cyanide content, and added a certain amount of saltpetre, improved the electroconductibility of silver plating solution;
3) improve concentration of silver ions, guaranteed that pulse moment has enough silver ionss to deposit at cathode surface, also helped improving the sedimentation velocity of silvering;
4) control of the content between each composition allows bigger variation range, and the content of especially free cyanogen need not strict control;
5) silvering grain refining, amount of hydrogen infiltration and impurity absorption are few, and silvering is highly polished, internal stress is low, microhardness is high, wear resistance is better and the anti-variable color time is long.
Embodiment
Further specify the present invention below by embodiment.
The test piece material of test usefulness is brass (H62), and the test piece specification is 50 * 100 * 3mm, and sample is divided into 4 group #, it is the conventional DC cyaniding plant of silver that every group of sample number is 3, the 4 groups: Silver Nitrate 40g/L, potassium cyanide 90g/L, salt of wormwood 15g/L, current density 0.5A/dm 2The double-pulse plating pulse waveform is a square wave.
It is as follows to use the silver plated technical process of two pulse:
A copper and copper alloy two pulse silver plating process flow process: weak etch, 5 pre-etch, 3 1) electrochemical degreasing, 2)) bright pickling, 4)) neutralization, 6) pre-copper facing, 7) two pulse silver-plated, 8) dehydration, 9) dry, 10) thermal treatment;
The technical process explanation:
1) electrochemical degreasing: workpiece is containing sodium hydroxide (NaOH) 5g/L～15g/L, sodium phosphate (Na 3PO 412H 2O) 30g/L～60g/L, yellow soda ash (Na 2CO 310H 2O) 20g/L～25g/L, water glass 3g/L～5g/L is in 60 ℃～80 ℃ aqueous solution of total alkalinity (being equivalent to NaOH) 15g/L～30g/L, with current density 1A/dm 2～5A/dm 2, the fuel-displaced 3min～10min of first negative electrode, anode oil removing≤30s again;
2) pre-etch: immerse in hydrochloric HCl (density 1.19) 50% (volume ratio) aqueous solution 0.5min～2min;
3) bright pickling: immerse chromic anhydride (CrO 3) 100g/L～150g/L, sulfuric acid H 2SO 45s～15s in the aqueous solution of (density 1.84) 20g/L～30g/L;
4) weak etch: 0.5min～2min in the aqueous solution of immersion hydrochloric acid (HCl) 100g/L～150g/L;
5) neutralization: immerse yellow soda ash (Na 2CO 310H 2O) 1min～2min in the aqueous solution of 30g/L～50g/L;
6) pre-copper facing, adopt pulse copper facing: sodium hydroxide (NaOH) 10g/L～20g/L, cuprous cyanide (CuCN) 35g/L～40g/L, sodium cyanide (NaCN) (always) 55g/L～65g/L, sodium cyanide (NaCN) (dissociating) 18g/L～22g/L aqueous solution, Mean Forward Current density: 0.4A/dm 2～1A/dm 2, forward conduction time: 0.2ms～0.4ms, cycle: 0.8ms～1.1ms, time: 8min～15min;
7) two pulse is silver-plated
8) dehydration: 100% dehydrated alcohol CH 3CH 2Soak 30s～60s among the OH;
9) drying, pressurized air dries up
10) thermal treatment: silver plate is put into baking oven for heating to 250 ℃ ± 10 ℃ of insulation 1h～1.5h, air cooling.
Embodiment 1
Be formulated as follows the silver plating solution of composition:
Saltpetre KNO 360g/L
Silver chloride AgCl 70g/L
Potassium cyanide KCN (always) 180g/L
Potassium cyanide KCN (dissociating) 110g/L
Get the 1st group of sample and electroplate, processing parameter is:
??i + m(A/dm 2) ??0.5
??i - m(A/dm 2) ??0.25
??T(ms) ??0.8
??t + on(ms) ??0.2
??t - on(ms) ??0.1
Positive negative pulse stuffing wave number ratio ??32∶8
Direct impulse work ratio ??0.1
Negative-going pulse work ratio ??0.05
Embodiment 2
Be formulated as follows the silver plating solution of composition:
Saltpetre KNO 380g/L
Silver chloride AgCl 75g/L
Potassium cyanide KCN (always) 180g/L
Potassium cyanide KCN (dissociating) 120g/L
Get the 2nd group of sample and electroplate, processing parameter is:
??i + m(A/dm 2) ??1.0
??i - m(A/dm 2) ??0.4
??T(ms) ??1.2
??t + on(ms) ??0.4
??t - on(ms) ??0.2
Positive negative pulse stuffing wave number ratio ??32∶6
Direct impulse work ratio ??0.2
Negative-going pulse work ratio ??0.1
Embodiment 3
Be formulated as follows the silver plating solution of composition:
Saltpetre KNO 3100g/L
Silver chloride AgCl 80g/L
Potassium cyanide KCN (always) 190g/L
Potassium cyanide KCN (dissociating) 120g/L
Get the 3rd group of sample and electroplate, processing parameter is:
??i + m(A/dm 2) ??1.5
??i - m(A/dm 2) ??0.5
??T(ms) ??1.5
??t + on(ms) ??0.4
??t - on(ms) ??0.2
Positive negative pulse stuffing wave number ratio ??32∶4
Direct impulse work ratio ??0.25
Negative-going pulse work ratio ??0.2
Coating performance detects
Visual inspection: at natural scattered beam or be bordering under the white light source of natural scattered beam and check that with 10 times of magnifying glasses the result is as follows:
Specimen coding ??1 ??2 ??3 ??4
Outward appearance Coating is careful, bright Coating is careful, bright Coating is careful, bright Coating is careful, matt
Thickness of coating detects, and the section of materialsing is surveyed the silvered film thickness that it is parallel to the matrix direction, and the result is as follows:
Specimen coding ??1 ??2 ??3 ??4
Thickness (μ m) ??22 ??27 ??32 ??18
Combining power test, carry out conventional DC silvered film and two pulse silvered film bonding force detection test by GB GB12307.2-90 requirement: stripping test and burnishing test, the result is as follows:
Specimen coding ??1 ??2 ??3 ??4
Bonding force Qualified Qualified Qualified Qualified
Ferroxyl test, test piece are incubated 1 hour under 250 ℃ of temperature, it is (individual/15cm to detect the silvering porosity again 2), porosity detects test and measures by being coated with the cream method, and the result is as follows:
Specimen coding ??1 ??2 ??3 ??4
Porosity is (individual/cm 2) ??0.24 ??0.25 ??0.20 ??0.73
Wear test, test piece are incubated 1 hour under 250 ℃ of temperature, detect wear loss, wear loss unit's (mg/100 time).Test conditions is: 360# sand paper, 200 gram load, past regrinding 1000 times.Testing tool: NUS-ISO-1 type wear testing machine, the result is as follows:
Specimen coding ??1 ??2 ??3 ??4
Wear loss (mg/100 time) ??3.72 ??3.75 ??3.68 ??4.28
Hardness detects, and the section of materialsing is surveyed the silvered film microhardness that it is parallel to the matrix direction, and test conditions is: 50 gram load; Testing tool: microhardness tester, the result is as follows:
Specimen coding ??1 ??2 ??3 ??4
Vickers' hardness (hv) ??110 ??109 ??119 ??88
The anti-discolouring test is placed on observation silvered film anti-tarnishing ability in the atmosphere with test piece, and the result is as follows:
Specimen coding ??1 ??2 ??3 ??4
Time (h) ??240 ??228 ??240 ??48
Internal stress detects, and adopts spiral taseometer test coating internal stress, and the result is as follows:
Specimen coding ??1 ??2 ??3 ??4
Average tension stress value (Kg/cm 2) ??1.30 ??1.26 ??1.25 ??3.5
Grain fineness number detects: dc plating silver layer and pulse plating silver layer amplify 7500 times, 15000 times Electronic Speculum pictures and grain-size detects by observing, the silver-plated grain-size 2-5 μ of conventional DC m, the silver-plated grain-size 0.1-0.2 μ of two pulse m, the silver-plated grain-size of two pulse has only about 1/25th of the silver-plated grain-size of conventional DC; The conventional DC silvered film is evenly distributed, crystal grain is thick, grain size differs; Pulse plating silver layer deposition compact, be evenly distributed, with coccoid particle deposition, tiny, the homogeneous grain size of crystal grain.

Claims (7)

1. plating silver solution, solvent is a water, the consisting of of solution:
Saltpetre KNO 3: 60g/L～100g/L
Silver chloride AgCl:70g/L～80g/L
Potassium cyanide KCN (always): 180g/L～190g/L
Potassium cyanide K CN (dissociating): 110g/L～120g/L
2. method of using the described solution of claim 1 to carry out double-pulse plating silver, electroplating technological parameter is:
Mean Forward Current density: 0.5A/dm 2～1.5A/dm 2
Negative sense average current density: 0.25A/dm 2～0.5A/dm 2
The forward conduction time: 0.2ms～0.4ms
Negative sense ON time: 0.1ms～0.2ms
The forward cycle: 0.8ms～1.5ms
The negative sense cycle: 0.8ms～1.5ms
Direct impulse work ratio: 0.1～0.25
Negative-going pulse work ratio: 0.05～0.2
Temperature: room temperature
3. the described double-pulse plating silver method of claim 2, described pulse waveform is a square wave.
4. the described double-pulse plating silver method of claim 2, described direct impulse: the preferable range of negative-going pulse is 32: 4～32: 8.
5. each double-pulse plating silver process in the use claim 2,3 or 4 mainly comprises the steps:
A copper and copper alloy two pulse silver plating process flow process: weak etch, 5 pre-etch, 3 1) electrochemical degreasing, 2)) bright pickling, 4)) neutralization, 6) pre-copper facing, 7) two pulse silver-plated, 8) dehydration, 9) dry, 10) thermal treatment;
B stainless steel two pulse silver plating process schema: weak etch, 4 pickling, 3 1) electrochemical degreasing, 2))) nickel preplating, 5) prepulsing silver-plated, 6) two pulse is silver-plated, 7) dry, 8) thermal treatment.
6. the described double-pulse plating silver process of claim 5, the preferred prepulsing copper facing of described pre-copper facing, composition and processing parameter are:
Sodium hydroxide NaOH:10g/L～20g/L
Cuprous cyanide CuCN:35g/L～40g/L
Sodium cyanide NaCN (always): 55g/L～65g/L
Sodium cyanide NaCN (dissociating): 18g/L～22g/L
Mean Forward Current density: 0.4A/dm 2～1A/dm 2
The forward conduction time: 0.2ms～0.4ms
Cycle: 0.8ms～1.1ms
Time: 8min～15min.
7. claim 5 or 6 described double-pulse plating silver process dewater and adopt 100% dehydrated alcohol.
CN200910060261A 2009-08-05 2009-08-05 Double-pulse plating silver solution and technique thereof Pending CN101629313A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102965701A (en) * 2012-12-18 2013-03-13 南通广联实业有限公司 Nickel-plating and silver-plating technology for tellurium copper
CN103255455A (en) * 2013-05-31 2013-08-21 东北大学 Method and device for pulse texturing treatment of surface of metal material
CN103382565A (en) * 2013-07-18 2013-11-06 扬州虹扬科技发展有限公司 Copper plating method and electroplating method of brass cast
CN103436931A (en) * 2013-08-26 2013-12-11 中国人民解放军第五七一九工厂 Bidirectional pulse silver-plating method
CN103668370A (en) * 2013-12-19 2014-03-26 潮州市连思科技发展有限公司 Method for pulse plating of disk
CN107119296A (en) * 2017-06-27 2017-09-01 中国人民解放军第五七九工厂 A kind of method of anode activation titanium alloy electro-coppering
CN108857273A (en) * 2018-06-13 2018-11-23 长春理工大学 A kind of 7075 superhydrophobic surface of aluminum alloy preparation processes
CN111118481A (en) * 2020-01-15 2020-05-08 中思缘环保科技有限公司 Full-automatic silver plating equipment and method
CN112323106A (en) * 2020-10-22 2021-02-05 深圳市海里表面技术处理有限公司 Rapid silver plating process
CN114934303A (en) * 2022-05-18 2022-08-23 江苏大学 Method and device for preparing local silver coating by laser-assisted electrochemical deposition technology

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102965701A (en) * 2012-12-18 2013-03-13 南通广联实业有限公司 Nickel-plating and silver-plating technology for tellurium copper
CN103255455A (en) * 2013-05-31 2013-08-21 东北大学 Method and device for pulse texturing treatment of surface of metal material
CN103382565A (en) * 2013-07-18 2013-11-06 扬州虹扬科技发展有限公司 Copper plating method and electroplating method of brass cast
CN103436931A (en) * 2013-08-26 2013-12-11 中国人民解放军第五七一九工厂 Bidirectional pulse silver-plating method
CN103668370A (en) * 2013-12-19 2014-03-26 潮州市连思科技发展有限公司 Method for pulse plating of disk
CN107119296A (en) * 2017-06-27 2017-09-01 中国人民解放军第五七九工厂 A kind of method of anode activation titanium alloy electro-coppering
CN108857273A (en) * 2018-06-13 2018-11-23 长春理工大学 A kind of 7075 superhydrophobic surface of aluminum alloy preparation processes
CN108857273B (en) * 2018-06-13 2021-08-31 长春理工大学 7075 aluminum alloy super-hydrophobic surface preparation process
CN111118481A (en) * 2020-01-15 2020-05-08 中思缘环保科技有限公司 Full-automatic silver plating equipment and method
CN112323106A (en) * 2020-10-22 2021-02-05 深圳市海里表面技术处理有限公司 Rapid silver plating process
CN114934303A (en) * 2022-05-18 2022-08-23 江苏大学 Method and device for preparing local silver coating by laser-assisted electrochemical deposition technology

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