CN101660182A - Trivalent chromium electroplate liquid stabilizer and electroplate liquid thereof - Google Patents
Trivalent chromium electroplate liquid stabilizer and electroplate liquid thereof Download PDFInfo
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- CN101660182A CN101660182A CN200910152494A CN200910152494A CN101660182A CN 101660182 A CN101660182 A CN 101660182A CN 200910152494 A CN200910152494 A CN 200910152494A CN 200910152494 A CN200910152494 A CN 200910152494A CN 101660182 A CN101660182 A CN 101660182A
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- trivalent chromium
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- stabilizer
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Abstract
The invention discloses a trivalent chromium electroplate liquid stabilizer and an electroplate liquid thereof, and is characterized in that the stabilizer is aqueous solvent formed by mixing 0.5 to 2mol/L methyl alcohol, 0.4 to 2.0 mol/L sodium sulfite and 0.5 to 2.5 mol/L ferrous sulfate; and the additive amount of the stabilizer is 1 to 30 ml per liter of the electroplate liquid. The inventionalso discloses a trivalent chromium electroplate liquid which fundamentally comprises the following components: 0.2 to 0.6 mol/L chromium sulfate, 0.5 to 1.5 mol/L potassium sulfate, 0.02 to 0.5 mol/L ammonium bromide, 0.5 to 1.2 mol/L boric acid, 0.2 to 0.5 mol/L sodium hypophosphite, 0.2 to 2.0 mol/L aminoacetic acid, 1 to 30 ml/L stabilizer and the balance of water which is used as solvent. The invention has the advantages that as the stabilizer is added into the trivalent chromium electroplate liquid, the stability and service life of the existing trivalent chromium electroplating technique are greatly improved; the plating has smooth and bright appearance, little cracks, good bonding force and lower cost; and the stabilizer can be widely applied in different trivalent chromium electroplating techniques.
Description
Technical field
The invention belongs to technical field of electrochemistry, relate to a kind of trivalent chromium plating liquid stablizer and electroplate liquid thereof.
Background technology
Promulgation on January 23rd, 2003 RoHS of European Parliament and board of management instruction regulation Europe is contained chromic electronic electric equipment in complete prohibition on July 1st, 2006 and is circulated in the European market; The EPA regulation will be completely forbidden the sexavalent chrome electroplating technology before 2010; China's " electronics and IT products pollution control management way " regulation is controlled chromic use since in March, 2007.Characteristics such as trivalent chromium plating is to substitute one of galvanized the most promising technology of sexavalent chrome, and it is little to have toxicity, only is one of chromic percentage, and energy consumption is low, dispersive ability and covering performance are good.The patent No. is that (Granted publication number: CN1042753C), plating bath is by 0.3-0.4mol/L CrCl in this patent for the Chinese invention patent " a kind of trivalent chromium plating liquid " of ZL94105903.0
36H
2O, 0.6-0.8mol/L HCOOH or HCOONH
4, 0.1-0.2mol/L NaBr, 0.8-1.0mol/L NaCl or KCl, 2.0-2.5mol/L NH
4Cl, 0.6-0.8mol/L H
3BO
3And proper amount of surfactant and rare earth addition composition, unavoidably will produce a large amount of chlorine and contaminate environment in this plating bath electroplating process, simultaneously, also there are deficiencies such as plating bath instability, coating color and luster are dark, crystallization velocity is slow, current efficiency is low." research of whole sulphate system trivalent chromium plating chromium " that " Wuhan University's journal (newspaper of science) " quick grade of the 50th volume the 2nd interim Wu Hui April in 2004 is shown has introduced sulfate trivalent chromium chrome-plated process and influence factor, and plating bath in the document (is unit with L) is composed as follows: Cr
2(SO
4)
36H
2O (25-50g), Na
2SO
4(100-150g), H
3BO
3(50-60g); complexing agent (20-25g); stablizer (20-25mL); brightening agent (5-10mL); but this bath stability is poor; again with reference to " sulfate system trivalent chromium plating technical study " that " material protection " June in 2007, the 40th volume the 6th interim Guan Yong etc. was shown; electroplate liquid in the document is made up of following component: open cylinder agent 80-140ml/L; conducting salt 280-340ml/L; auxiliary 8-12ml/L; wetting agent 2-4ml/L; cleaner 5-10ml/L; wherein open the coordination agent that the cylinder agent comprises chromium sulphate double salt and is made up of multiple carboxylic acid or carboxylate salt, conducting salt comprises boric acid; plurality of inorganic salt such as sodium sulphate, auxiliary contain multiple rare metal salts and comprise phenyl; the organism of groups such as-C ≡ C-.
Also have many open in the patent documentation, referring to application number is open " the chromed hardened method of the metallic substance " (publication number: CN1687486A) of 200510020382.5 Chinese invention patent application, chromed hardened plating bath chemical ingredients and concentration are as follows in this patent: chromic anhydride 220-280g/L, sulfuric acid 2.5-4.5g/L, trivalent chromium 1.5-7g/L, it referring to application number again 20061009033.6 Chinese invention patent application " a kind of trivalent chromium electroplating solution in sulfate system and preparation method " (publication number: CN1880512A), electroplate liquid is formulated by the component of following molar content in this patent: chromium sulphate 0.05-0.25mol/L, sodium sulfate 0.4-0.8mol/L, boron 0.7-1.2mol/L, Tai-Ace S 150 0.075-0.18mol/L, sodium lauryl sulphate 0.0001-0.004mol/L, complexing agent 0.2-1.0mol/L, stablizer 0.04-0.5mol/L, all the other are aqueous solvent.
One of subject matter of trivalent chromium plating existence at present is that coating can not continue to thicken, and the plating bath instability is low to the impurity tolerance, easily loses efficacy.Adopt stablizer can prevent the introducing of foreign ion, keep the stable of each component of plating bath, thereby improve the work-ing life and the electroplating quality of plating bath.The present invention develops a kind of trivalent chromium plating liquid and stablizer thereof exactly, can improve the stability of trivalent chromium plating greatly, advances its industrial applications.
Summary of the invention
First technical problem to be solved by this invention is to provide a kind of trivalent chromium plating liquid stablizer at the above-mentioned state of the art, use this stablizer can prevent that the plating bath active principle is oxidized, the dispersion inequality of constituents for suppressing keeps the stable of trivalent chromium plating technology for a long time.
Second technical problem to be solved by this invention provides a kind of trivalent chromium plating liquid, makes the stable performance life-span long, and quality of coating is good.
The technical scheme that the present invention is adopted for above-mentioned first technical problem of solution is: a kind of trivalent chromium plating liquid stablizer, it is characterized in that stablizer is the aqueous solution that following material is formed: 0.5-2mol/L methyl alcohol, 0.4-2.0mol/L S-WAT, the 0.5-2.5mol/L ferrous sulfate.
Described trivalent chromium plating liquid stablizer is used for trivalent chromium plating technology, and addition is every liter of electroplate liquid 1-30ml.
The present invention for above-mentioned second technical scheme that technical problem adopted of solution is: a kind of trivalent chromium plating liquid is characterized in that by the component of following volumetric molar concentration formulated:
Chromium sulphate 0.2～0.6mol/L;
Vitriolate of tartar 0.5～1.5mol/L;
Brometo de amonio 0.02～0.5mol/L;
Boric acid 0.5～1.2mol/L;
Inferior sodium phosphate 0.2～0.5mol/L;
Padil 0.2～2.0mol/L;
Stablizer 1～30ml/L;
All the other are aqueous solvent;
Described stablizer is the aqueous solution that following material is formed: 0.5-2mol/L methyl alcohol, 0.4-2.0mol/L S-WAT, 0.5-2.5mol/L ferrous sulfate.
The pH value of described trivalent chromium plating liquid is 2.0-3.5.
Technological temperature when described trivalent chromium plating liquid is electroplated is 30-40 ℃, and cathode current density is 5-20A/dm
2, bath pH value 2.0-3.5, electroplating time 1-10 minute, anode was a coated electrode.
Chromium sulphate provides chromium ion for plating bath in the trivalent chromium plating liquid formula component of the present invention, and vitriolate of tartar and brometo de amonio are conducting salt, is used for increasing the plating bath electricity and leads, and improves solution dispersibility and reduces power consumption; Boric acid is the plating bath buffer reagent, is used for keeping the pH value of plating bath in processing range; Padil and trivalent chromic ion complexing are converted into electroactive high easy deposition complex ion with inert trivalent chromium hydrate, to improve the sedimentation velocity and the current efficiency of plating bath, improve quality of coating; Boric acid can effectively be stablized the pH value of plating bath, keeps the stable of long-time electroplating bath solution acidity, guarantee coating continue thicken.Stablizer is used for preventing that trivalent chromic ion is oxidized to hexavalent chromium, simultaneously already present hexavalent chromium in the plating bath is reduced to trivalent chromic ion to improve the stability and the work-ing life of plating bath
Trivalent chromium plating liquid stablizer range of application of the present invention not only is confined to above-mentioned trivalent chromium plating liquid formula, can be widely used in the different trivalent chromium plating technology.
The present invention compared with prior art has the following advantages and effect:
1, the trivalent chromium plating liquid of the present invention development carries out in the chrome-plating process only precipitated oxygen of anode, cleanliness without any pollution, and coating outward appearance light, crackle is few, and bonding force is good, and raw material sources are abundant, and cost is lower, has excellent cost performance.
2, after stablizer of the present invention is introduced, effectively improve the stability of plating bath, help its industrialization promotion.
Embodiment
1, preparation trivalent chromium plating liquid stablizer:
0.5-2mol/L methyl alcohol;
0.4-2.0mol/L S-WAT;
0.5-2.5mol/L ferrous sulfate;
All the other components are water.
With above-mentioned starting material, uniform mixing gets final product in water.
2, preparation trivalent chromium plating liquid, formulated by the component of following volumetric molar concentration:
Chromium sulphate 0.2-0.6mol/L;
Vitriolate of tartar 0.5-1.5mol/L;
Brometo de amonio 0.02-0.5mol/L;
Boric acid 0.5-1.2mol/L;
Inferior sodium phosphate 0.2-0.5mol/L;
Padil 0.2-2.0mol/L;
The stablizer 1-30ml/L of step 1 preparation;
All the other are water.
Take by weighing starting material by said ratio, earlier that chromium sulphate is soluble in water; Then that boric acid is soluble in water, be stirred to dissolving, because the solubleness of boric acid in water is lower, so boric acid solution need be heated to 60-70 ℃ so that its whole dissolvings. then boric acid solution and chromium sulfate solution are mixed, stir, add Padil again, Padil should stir after adding fully, so that it generates the moderate electroactive complex ion of more stability.If trivalent chromium in the electroplate liquid and complexing agent complexing is bad, perhaps complexing agent concentration is too low, and the maximum current density that plating bath allows will reduce, or only obtains the dirt settling of black even do not have coating.So should make trivalent chromium and complexing agent complexing complete.
Add vitriolate of tartar subsequently, brometo de amonio, inferior sodium phosphate, stablizer.Vitriolate of tartar is a conducting salt, with the dispersive ability that improves plating bath and reduce power consumption.Brometo de amonio, inferior sodium phosphate has reductibility, and it is oxidized effectively to suppress trivalent chromic ion, strengthens the stability of plating bath.Boric acid in the plating bath has stronger pH value shock absorption, can effectively stablize the pH value of plating bath, and stablizer can be kept the stable of long-time electroplating process plating bath acidity, guarantee coating continue thicken.After all components all added, the pH that adjusts plating bath was to specialized range, and constant temperature fully stirred 1 hour then, left standstill then 1 hour so that the trivalent chromic ion complexing is complete, improved the stability of plating bath.
The processing parameter of electroplate liquid of the present invention is as follows: working temperature 30-40 ℃, and cathode current density 5-20A/dm
2, bath pH value 2.0-3.5, electroplating time 1-10min, anode are coated electrode.After pre-treatment cleaned, eliminates rust and activate before according to the plating of routine with workpiece, as negative electrode, the cathode and anode area was about 1: 2 with workpiece to be plated.
Below by embodiment, further illustrate outstanding feature of the present invention and marked improvement, only be the present invention is described and never limit the present invention.
Embodiment 1
Get 2mol methyl alcohol, 0.5mol S-WAT, 1mol ferrous sulfate are mixed with the 1000mL stablizer aqueous solution.
Get the chromium sulphate of 0.2mol, be dissolved in distilled water, be stirred to dissolving fully; The boric acid of getting 0.5mol is soluble in water, is stirred to dissolving; Above-mentioned gained chromium sulfate solution is mixed with boric acid solution, stir; Add brometo de amonio and the Padil of 0.5mol, stirred 0.5 hour, add the 0.5mol vitriolate of tartar subsequently successively, the 0.3mol inferior sodium phosphate.Add the 5ml stablizer aqueous solution at last, add adding water near 1L; The pH value that detects, adjusts solution then is 2.0; Temperature control is 30 ℃ behind the constant volume, after pre-treatment cleans, eliminates rust and activate before according to the plating of routine with workpiece, at 10A/dm
2Electroplated under the current density 3 minutes, and took out the back water and rinse well, promptly obtain bright smooth about thickness 2 μ m, flawless trivalent chromium hard chromium after test piece is done.
Embodiment 2
Get 0.5mol methyl alcohol, 0.4mol S-WAT, 0.5mol ferrous sulfate are mixed with the 1000mL stablizer aqueous solution.
Get the chromium sulphate of 0.6mol, water-soluble, be stirred to dissolving; The boric acid of getting 0.8mol is dissolved in the distilled water, is stirred to dissolving; Above-mentioned gained chromium sulfate solution is mixed with boric acid solution, stir; Add the 2.0mol Padil, stirred 1 hour, add the 1.0mol vitriolate of tartar subsequently successively, the 0.5mol inferior sodium phosphate at 55 ℃, 0.2mol brometo de amonio, the 30ml stablizer aqueous solution, the limit edged stirs, until dissolving, constant temperature stirred static 1 hour 1 hour for 60 ℃ subsequently; Add and add water near 1L; The pH value that detects, adjusts solution then is 3.0; Temperature control is 40 ℃ behind the constant volume, and workpiece is passed through degreasing, washing, acid etching successively, and washing is at 15A/dm
2Electroplated 8 minutes under the current density, take out back water flushing, promptly obtain smooth trivalent chromium hard chromium.
Embodiment 3
Get 1mol methyl alcohol, 2mol S-WAT, 2.5mol ferrous sulfate are mixed with the 1000mL stablizer aqueous solution.Add the 1ml/L stablizer every day before embodiment 1 electroplating solution work, can keep the stable long-play of electroplating technology.
Embodiment 4
Get 0.5mol methyl alcohol, 0.4mol S-WAT, 2.5mol ferrous sulfate are mixed with the 1000mL stablizer aqueous solution.With the chromium sulphate of 0.4mol, water-soluble, 1.0mol boric acid is water-soluble, the 1.5mol Padil, 1.5mol vitriolate of tartar, the 0.4mol inferior sodium phosphate, the 0.5mol brometo de amonio mix to stir until dissolving, 55 ℃ were stirred 2 hours, added the stablizer that 15ml has prepared, and added adding water near 1L; The pH value of adjusting solution is 3.5, and 40 ℃ of temperature controls pass through degreasing, washing, acid etching successively with workpiece, and washing is at 10A/dm
2Electroplated 5 minutes under the current density, taking-up is rinsed well, drying.This trivalent chromium plating liquid good stability, the life-span is long, has broad application prospects.
In a word, the trivalent chromium plating solution stable performance life-span of the present invention is long, and quality of coating is good, stabilizing agent of the present invention, energy Greatly improve technology stability and the quality of coating of plating bath, have good application prospect and use value.
Claims (5)
1, a kind of trivalent chromium plating liquid stablizer is characterized in that stablizer is the aqueous solution that following material is formed: 0.5-2mol/L methyl alcohol, 0.4-2.0mol/L S-WAT, 0.5-2.5mol/L ferrous sulfate.
2, a kind of trivalent chromium plating liquid stablizer according to claim 1 is characterized in that stablizer is used for trivalent chromium plating technology, and addition is every liter of electroplate liquid 1～30ml.
3, a kind of trivalent chromium plating liquid is characterized in that comprising following component and corresponding volumetric molar concentration proportioning:
Chromium sulphate 0.2～0.6mol/L;
Vitriolate of tartar 0.5～1.5mol/L;
Brometo de amonio 0.02～0.5mol/L;
Boric acid 0.5～1.2mol/L;
Inferior sodium phosphate 0.2～0.5mol/L;
Padil 0.2～2.0mol/L;
Stablizer 1～30ml/L;
All the other are aqueous solvent;
Described stablizer is the aqueous solution that following material is formed: 0.5-2mol/L methyl alcohol, 0.4-2.0mol/L S-WAT, 0.5-2.5mol/L ferrous sulfate.
4, a kind of trivalent chromium plating liquid according to claim 3 is characterized in that described electroplate liquid pH value is 2.0-3.5.
5, a kind of trivalent chromium plating liquid according to claim 3, it is characterized in that the processing parameter of described electroplate liquid is: technological temperature is 30-40 ℃, cathode current density is 5-20A/dm
2, bath pH value 2.0-3.5, electroplating time 1-10 minute, anode was a coated electrode.
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| CN103898561A (en) * | 2013-06-03 | 2014-07-02 | 无锡市锡山区鹅湖镇荡口青荡金属制品厂 | Electric-plating solution for plating nickel on surface of magnesium alloy die-cast piece |
| CN103898560A (en) * | 2013-06-03 | 2014-07-02 | 无锡市锡山区鹅湖镇荡口青荡金属制品厂 | Electroplating process for chrome plating on surface of magnesium alloy pressure casting |
| CN104388989A (en) * | 2014-11-14 | 2015-03-04 | 无锡信大气象传感网科技有限公司 | Trivalent chromium electroplating liquid and preparation method thereof |
| CN104894611A (en) * | 2015-06-10 | 2015-09-09 | 陈新棠 | Electroplating liquid stabilizing agent |
| CN105018974A (en) * | 2015-08-21 | 2015-11-04 | 无锡桥阳机械制造有限公司 | Trivalent chromium electroplate liquid and preparing method thereof |
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| CN105239111A (en) * | 2015-10-29 | 2016-01-13 | 无锡桥阳机械制造有限公司 | Trivalent chromium electroplate liquid and preparing method thereof |
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- 2009-09-10 CN CN200910152494A patent/CN101660182A/en active Pending
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| CN103898560A (en) * | 2013-06-03 | 2014-07-02 | 无锡市锡山区鹅湖镇荡口青荡金属制品厂 | Electroplating process for chrome plating on surface of magnesium alloy pressure casting |
| CN103898561A (en) * | 2013-06-03 | 2014-07-02 | 无锡市锡山区鹅湖镇荡口青荡金属制品厂 | Electric-plating solution for plating nickel on surface of magnesium alloy die-cast piece |
| CN104388989A (en) * | 2014-11-14 | 2015-03-04 | 无锡信大气象传感网科技有限公司 | Trivalent chromium electroplating liquid and preparation method thereof |
| CN104894611A (en) * | 2015-06-10 | 2015-09-09 | 陈新棠 | Electroplating liquid stabilizing agent |
| CN105063680A (en) * | 2015-08-21 | 2015-11-18 | 无锡桥阳机械制造有限公司 | Sulfonic acid type semi-bright pure-tin electroplating liquid |
| CN105018974A (en) * | 2015-08-21 | 2015-11-04 | 无锡桥阳机械制造有限公司 | Trivalent chromium electroplate liquid and preparing method thereof |
| CN105239111A (en) * | 2015-10-29 | 2016-01-13 | 无锡桥阳机械制造有限公司 | Trivalent chromium electroplate liquid and preparing method thereof |
| CN105332009A (en) * | 2015-11-16 | 2016-02-17 | 张颖 | Sulphate-system environment-friendly electroplating method |
| CN105401176A (en) * | 2015-11-16 | 2016-03-16 | 张颖 | Sulfate-system environment-friendly electroplating solution |
| CN109137002A (en) * | 2018-11-09 | 2019-01-04 | 施泰尔精密机械（常熟）有限公司 | A kind of heavy parts Cr-plating Bath |
| CN111676494A (en) * | 2020-07-16 | 2020-09-18 | 上海交通大学 | Trivalent chromium electroplating solution, preparation method and application |
| CN111850621A (en) * | 2020-07-16 | 2020-10-30 | 上海交通大学 | Trivalent chromium electroplating solution and preparation method thereof |
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Open date: 20100303 |