CN102443825B - High-concentration chromium sulfate-ammonium fluoride trivalent chromium electroplating solution and preparation method thereof - Google Patents
High-concentration chromium sulfate-ammonium fluoride trivalent chromium electroplating solution and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high concentration chromium sulfate-ammonium fluoride trivalent chromium electroplating solution and a preparation method thereof. The preparation method comprises steps that: (10 pure water with a volume of 2/3 of that a preset total electroplating solution volume is added into a vessel, and is heated; 30-70g/L of a buffering agent boric acid is added to the water, and is dissolved by stirring; (2) 60-150g/L of sodium chloride, 50-100g/L of ammonium chloride, 30-80g/L of ammonium fluoride, and 8-10g/L of ammonium bromide are added to the solution, and are dissolved by stirring; (3) 30-50g/L of an auxiliary complexing agent is added to the solution, and is dissolved by stirring; the pH value of the solution is regulated to 2.5-3.0; (4) 110-210g/L of a main salt chromium sulfate is added to the solution, and is dissolved by stirring; the pH value of the solution is regulated to 2.8-3.0; (5) 0.1-0.5g/L of polyethylene glycol is added to the mixture; pure water is added until a full dose is reached; the temperature is maintained at 55-60 DEG C; and aging is carried out for more than 12 hours with the maintained temperature, such that a finished product is obtained. According to the invention, advantages of two technological systems which are a total-sulfate system and a chloride system are integrated and optimized. An obtained chrome plating layer is uniform, white, and bright. The displacement is wide, and a full-bright decorative effect is achieved. The current efficiency of the electroplating solution is high, and the deposition speed of the electroplating solution is high. Therefore, with the electroplating solution, an obtained effect is better than that with a common total-sulfate trivalent chromium electroplating technological system in markets.
Description
(i) technical field: the present invention relates to a kind of trivalent chromium plating solution and preparation method thereof; A kind of high-concentration chromium sulfate-ammonium fluoride trivalent chromium electroplating solution and preparation method thereof specifically; The present invention can be widely used in the surface decoration chromium plating of the component such as machinery, electronics, electrical equipment, instrument, automobile, to improve the solidity to corrosion of these component and ornamental.
(ii) background technology: chromium coating has higher hardness and good wear resistance, solidity to corrosion, ornamental because of it, therefore being widely used in the protecting decorative coating of the component such as machinery, electronics, electrical equipment, instrument, automobile, household electrical appliances, is one of most widely used plating of electroplating industry.The electroplating process that obtains at present chromium coating mainly contains two kinds, and a kind of is traditional hexavalent chromium plating technique, and another kind is trivalent chromium plating Technology.The toxicity of producing due to hexavalent chromium plating is large, and pollute and weigh, wastewater treatment difficulty, the water source causing, soil and air environmental pollution, caused the great attention of countries in the world; For example European Parliament promulgates that the electric equipment products of ROHS instruction regulation complete prohibition on July 1st, 2006 hexavalent chromium plating is used in European market, and EPA completely forbids hexavalent chromium plating and produces before being defined in 2010; China also proposes very strict requirement to chromic production discharge about the environmental regulation of cleaner production.In order to replace hexavalent chromium plating technique, people have carried out large quantity research to the lower trivalent chromium plating of toxicity.The trivalent chromium plating technique of using in Electroplating Production at present mainly contains two individual system, and a kind of is whole sulphate process system, and a kind of is chloride process system.It is high similar to sexavalent chrome coating color and luster that whole sulphate process system has coating white luminance, anode be take oxygen evolution reaction as the less advantage of main environmental pollution degree, but the main salt metal content of whole sulphate process system ubiquity plating solution is low, bath stability is poor, current efficiency is low, sedimentation velocity is slow, short bath maintenance of production feed supplement cycle is adjusted complicated loaded down with trivial details shortcoming, and chromic oxidation very easily occurs Oxygen anodic evolution, generate sexavalent chrome contaminating impurity and cause plating solution to stop production and lost efficacy; Therefore whole sulphate process system generally adopts precious metal to film anode to suppress chromic generation, or adds reducing substances to eliminate chromic accumulation; But precious metal is filmed, the input cost of anode is short high work-ing life, and the reducing substance adding also can final oxidized formation impurities accumulation and affected the normal production of plating solution, so the less use in actual Electroplating Production of whole sulphate trivalent chromium process system.And in electroplating actual production, use more muriate trivalent chromium process system at present, there is anode to separate out the shortcoming that chlorine affects production environment, and the white luminance of gained coating is also not as whole sulphate process system; But the main salt metal content of chloride system is higher, plating solution production stability is good, the high sedimentation velocity of current efficiency is fast, in electroplating process, generally can not generate sexavalent chrome impurity, and can use graphite anode production cost low, so muriate trivalent chromium process system obtains more application in actual Electroplating Production.
(iii) summary of the invention: the object of the present invention is to provide a kind of high-concentration chromium sulfate-ammonium fluoride trivalent chromium electroplating solution and preparation method thereof; Complex optimum of the present invention the advantage of whole sulphate and two process systems of muriate, adopt high-concentration sulfuric acid chromium as main salt, kept sulfate trivalent chromium to electroplate the high characteristic of gained coating white luminance, in appearance luster, be better than muriate trivalent chromium process system; Adopt chlorate as conducting salt, improved the electroconductibility of plating solution, kept the fast advantage of the high sedimentation velocity of chloride process system current efficiency; By optimization, screen and using Neutral ammonium fluoride as main complexing agent, improved the concentration of trivalent chromium complex ion in plating solution, make plating solution have advantages of that the good stability production feed supplement cycle is long; And on electroplate liquid formulation forms, broken the routine that current trivalent chromium plating technical field generally adopts organic monoacid salt coordination chromium ion, made this formula there is clear superiority on actual electroplating effect.Gained chromium coating of the present invention is evenly bright in vain, walks broad, reaches complete bright decorative effect; The high sedimentation velocity of plating solution current efficiency is fast, is better than the whole sulphate trivalent chromium plating process system generally using on market.
A kind of high-concentration chromium sulfate-ammonium fluoride trivalent chromium electroplating solution of the present invention, its plating solution consists of: chromium sulphate 110-210 grams per liter is (with Cr
2(SO
4)
36H
2o meter), sodium-chlor 60-150 grams per liter, ammonium chloride 50-100 grams per liter, boric acid 30-70 grams per liter, Neutral ammonium fluoride 30-80 grams per liter, brometo de amonio 8-10 grams per liter, auxiliary complex-former carboxylate salt total amount is 30-50 grams per liter, wetting agent polyoxyethylene glycol 0.1-0.5 grams per liter, and all the other are aqueous solvent.
The processing parameter of described electroplate liquid is: working temperature 20-40 ℃, cathode current density 10-20A/dm
2, bath pH value 2.5-3.2, electroplating time 2-15 minute, anode is graphite anode.
Described auxiliary complex-former carboxylate salt is comprised of two kinds low molecule organic monoacid salt, and a class is selected from a kind of in the ammonium salt of formic acid, acetic acid, oxalic acid, Padil or sodium salt, a kind of in the another kind of salt that is selected from tartrate, oxysuccinic acid, citric acid, EDTA; The 1.5-2 that wherein, the consumption of the low molecule organic monoacid of class salt is last class doubly.
The method of preparing above-mentioned a kind of high-concentration chromium sulfate-ammonium fluoride trivalent chromium electroplating solution, comprises the steps:
(1) the pure water that first adds predetermined total plating solution volume 2/3 in plating tank, is heated to 55-60 ℃, then adds buffer reagent boric acid, stirs completely and dissolves;
(2) add respectively conducting salt sodium-chlor, ammonium chloride, main complexing agent Neutral ammonium fluoride, anodic inhibitor brometo de amonio, stirs completely and dissolves;
(3) add auxiliary complex-former, stir after dissolving completely, the pH value of adjusting solution with concentrated hydrochloric acid is 2.5-3.0;
(4) add and become owner of salt chromium sulphate, stir after dissolving completely, the pH value of adjusting solution with massfraction 20%NaOH solution is 2.8-3.0;
(5) add wetting agent polyoxyethylene glycol, supplement pure water to predetermined total plating solution volume; Keeping the temperature of plating solution is 55-60 ℃, is incubated ageing more than 12 hours.
The present invention has following features:
1. adopt the chromium sulphate of high density as electroplating main salt, with higher metal chromium ions content, improve current efficiency and the sedimentation velocity of electroplate liquid, the production feed supplement cycle that extends plating solution is improved production stability, has kept gained chromium coating to have advantages of that the careful white luminance of sulfate process system crystallization is high simultaneously.Gained chromium coating is better than muriate trivalent chromium process system in decorative appearance.
2. adopt sodium-chlor ammonium chloride as conducting salt, have than the fast electrochemistry advantage of the high sedimentation velocity of general whole sulphate trivalent chromium bath good conductivity current efficiency, in actual production, raise the efficiency energy-saving and cost-reducing.Because halide-ions has precedence over the discharge oxidation of trivalent chromic ion on anode, thereby effectively suppressed trivalent chromium, be oxidized to chromic electrode process, eliminated the hidden danger of sexavalent chrome impurity to plating solution pollution failure.
3. preferably composite by multiple complexing agent, developed and a kind ofly usingd Neutral ammonium fluoride as main complexing agent, low molecular carboxylic acid salt is as the solution system of auxiliary complex-former, make in plating solution of the present invention the formed multicomponent complex of trivalent chromic ion there is electrochemical stability moderate, high low area current potential equalization discharge walks broad, the consistent advantage of the good color and luster of gained coating uniformity, and can be when the higher and change in concentration of main salt content of chromium ion be larger (23 ~ 45 grams per liter) obtain the chromium coating of good appearance.
4. adopt the boric acid generally using as buffer reagent, and in plating solution the shock-absorbing capacity of the anti-pH value variation of comprehensive performance under the synergy of other organic monoacid salt, effectively guaranteed the production stability that the anti-pH value of plating solution changes, making electroplating time can extend coating can thicken.
5. adopt low-molecular-weight polyethylene glycol (polymerization degree 200 ~ 400) as wetting agent, coating of the present invention is had to promoter action, show as compact crystallization degree and the luminance brightness of obvious raising chromium coating, strengthened the decorative appearance effect of chromium coating.
6. adopt graphite anode to reduce Electroplating Production cost; The present invention does not generate harmful sexavalent chrome impurity in plating production process, and therefore having solved whole sulphate trivalent chromium plating generally can not use the technical barrier of graphite anode.
The present invention compared with prior art, has the following advantages and effect:
1. the trivalent chromium plating solution employing high-concentration sulfuric acid chromium of the present invention's development is main salt, chromium metal concentration can reach 45 grams per liters, be 3 ~ 10 times of general whole sulphate trivalent chromium plating solution, thereby extended the plating solution production feed supplement cycle and improved stability and the working efficiency of Electroplating Production.
2. to adopt halogenide be conducting salt in the present invention, and than the good conductivity of whole sulphate trivalent chromium process system, the high sedimentation velocity of current efficiency is fast; Electroplating process middle slot loss of voltage power consumption reduces, energy-saving and cost-reducing in actual production.And the halide-ions adding has changed the Electrode behaviour of analysing oxygen on anode, effectively suppress trivalent chromic ion and be oxidized to chromic phenomenon, therefore can not use the expensive precious metal anode of filming, also need not add reducing substances to suppress chromic accumulation.
3. take inorganic salt Neutral ammonium fluoride as main complexing agent can be so that chromium sulphate keeps good plating adaptability under higher concentration, its actual effect is as previously mentioned.And the whole sulphate trivalent chromium technique that research is used at present, generally adopt organic carboxylate as main complexing agent, and when chromium sulphate main salt concentration is lower (common metal chromium 4-10 grams per liter), could realize the practical application performance of plating solution, thereby the present invention has obvious practical advantages.
4. the wide ranges good stability life cycle that the anti-pH of plating solution changes is long, and plating solution use temperature is low can work at normal temperatures, and technological operation is easy.
5. the present invention adopts graphite anode Electroplating Production cost low, does not produce harmful sexavalent chrome impurity in electroplating process, therefore than whole sulphate trivalent chromium process system, has obvious practicality advantage.
6. the electroplating bath components of the present invention's development is simple, and raw material market is in liberal supply, aboundresources, and cost is lower, has excellent cost performance, and market application foreground is wide.
(iv) embodiment:
Specific embodiments of the invention are as follows:
The raw material of 6 six kinds of trivalent chromium plating solutions of embodiment 1-embodiment forms and consumption (take and prepare 1 liter of electroplate liquid as example explanation) is as shown in table 1, by 6 six kinds of electroplate liquids of embodiment 1-embodiment, with Hull Cell, tests to check its serviceability; Prepare sexavalent chrome standard Cr-plating Bath simultaneously and carry out Hull Cell experiment with as a comparison, its result is as shown in table 2.
The content of sexavalent chrome standard Cr-plating Bath is: chromic anhydride 250 grams per liters, sulfuric acid 2.5 grams per liters, trivalent chromium 3 grams per liters.
The raw material of table 1 embodiment 1-6 trivalent chromium plating solution forms and consumption
Embodiment 1-6 trivalent chromium plating liquid making method is as follows:
(1) the pure water that first adds predetermined total plating solution volume 2/3 in plating tank, is heated to 55-60 ℃, then adds buffer reagent boric acid, stirs completely and dissolves;
(2) add according to quantity respectively conducting salt sodium-chlor, ammonium chloride, main complexing agent Neutral ammonium fluoride, anodic inhibitor brometo de amonio, stirs completely and dissolves;
(3) add according to quantity a kind of in formic acid, acetic acid, oxalic acid, Padil, then add according to quantity a kind of in oxysuccinic acid, tartrate, citric acid, EDTA, after stirring and dissolving completely, the pH value of adjusting solution with concentrated hydrochloric acid is 2.5 ~ 3.0;
(4) add according to quantity and become owner of salt chromium sulphate, stir after dissolving completely, the pH value of adjusting solution with massfraction 20%NaOH solution is 2.8-3.0;
(5) add according to quantity wetting agent polyoxyethylene glycol, supplement pure water to predetermined total plating solution volume; Keeping the temperature of plating solution is 55-60 ℃, is incubated ageing more than 12 hours.
Table 2 embodiment 1-6 electroplate liquid and sexavalent chrome standard plating solution Hull Cell experimental result
Hull Cell current density range calculation formula is pressed:
D
k=I(5.1-5.24lgL) L=0.1~8.8cm
The Hull Cell anode of the embodiment 1 ~ 6 of trivalent chromium bath adopts graphite cake anode, and the Hull Cell anode of sexavalent chrome plating solution adopts stereotype.Negative electrode test piece all adopts the latten(-tin) (100 * 65 millimeters) of 0.5 millimeter of thickness, and test piece is processed with 360# liquid honing before electroplating.
From the experimental result shown in table 2, can find out, the trivalent chromium plating solution of the different concns of embodiment 1 ~ 6 all has broad bright district current density range, demonstrate electroplate liquid of the present invention and there is good walking property, and can change under condition greatly at main salt concentration and other concentration of component, obtain the bright coating of Deposit appearance uniformity.With the contrast of sexavalent chrome standard plating solution, the luminance brightness of its dispersive ability of electroplate liquid of the present invention and walking property and Deposit appearance all will surmount traditional hexavalent chromium plating.Prove that thus trivalent chromium plating solution provided by the present invention has good use properties.
It should be noted that, above-described embodiment 1-6 is just to brief description of the present invention, rather than limitation of the present invention, does not anyly exceed the intraparenchymatous innovation and creation of the present invention, all falls within the scope of protection of the present invention.
Claims (4)
1. a high-concentration chromium sulfate-ammonium fluoride trivalent chromium electroplating solution, is characterized in that plating solution consists of: chromium sulphate 110-210 grams per liter is with Cr
2(SO
4)
36H
2o meter, sodium-chlor 60-150 grams per liter, ammonium chloride 50-100 grams per liter, boric acid 30-70 grams per liter, Neutral ammonium fluoride 30-80 grams per liter, brometo de amonio 8-10 grams per liter, auxiliary complex-former carboxylate salt total amount is 30-50 grams per liter, wetting agent polyoxyethylene glycol 0.1-0.5 grams per liter, and all the other are aqueous solvent.
2. a kind of high-concentration chromium sulfate-ammonium fluoride trivalent chromium electroplating solution according to claim 1, is characterized in that: the processing parameter of described electroplate liquid is: working temperature 20-40 ℃, cathode current density 10-20A/dm
2, bath pH value 2.5-3.2, electroplating time 2-15 minute, anode is graphite anode.
3. a kind of high-concentration chromium sulfate-ammonium fluoride trivalent chromium electroplating solution according to claim 1 and 2, it is characterized in that: described auxiliary complex-former carboxylate salt is comprised of two kinds low molecule organic monoacid salt, a kind of in a kind of ammonium salt that is selected from formic acid, acetic acid, oxalic acid, Padil or sodium salt, another kind is selected from a kind of in the salt of tartrate, oxysuccinic acid, citric acid, EDTA; The 1.5-2 that wherein, the consumption of the low molecule organic monoacid of class salt is last class doubly.
4. the preparation method of a kind of high-concentration chromium sulfate-ammonium fluoride trivalent chromium electroplating solution as claimed in claim 1, is characterized in that comprising the steps:
(1) the pure water that first adds predetermined total plating solution volume 2/3 in plating tank, is heated to 55-60 ℃, then adds buffer reagent boric acid, stirs completely and dissolves;
(2) add respectively conducting salt sodium-chlor, ammonium chloride, main complexing agent Neutral ammonium fluoride, anodic inhibitor brometo de amonio, stirs completely and dissolves;
(3) add auxiliary complex-former, stir after dissolving completely, the pH value of adjusting solution with concentrated hydrochloric acid is 2.5-3.0;
(4) add and become owner of salt chromium sulphate, stir after dissolving completely, the pH value of adjusting solution with massfraction 20%NaOH solution is 2.8-3.0;
(5) add wetting agent polyoxyethylene glycol, supplement pure water to predetermined total plating solution volume; Keeping the temperature of plating solution is 55-60 ℃, is incubated ageing more than 12 hours.
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| CN103510130B (en) * | 2012-06-26 | 2016-08-24 | 武汉材料保护研究所 | Trivalent hard chromium electro-plating method |
| CO7190036A1 (en) * | 2014-02-11 | 2015-02-19 | Garcia Carlos Enrique Muñoz | Continuous trivalent chrome plating process |
| 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 |
| CN105696028A (en) * | 2014-11-28 | 2016-06-22 | 中国科学院金属研究所 | Trivalent chromium electroplating solution and electroplating method |
| 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 |
| CN106521610B (en) * | 2016-12-22 | 2018-07-13 | 西安博岳环保科技有限公司 | A kind of hexavalent chromium plating combination Ni―Ti anode and preparation method thereof |
| CN111349952B (en) * | 2020-03-06 | 2021-06-08 | 广州三孚新材料科技股份有限公司 | Trivalent black chromium electroplating solution for solar heat collector |
| FR3110606A1 (en) * | 2020-05-20 | 2021-11-26 | Institut De Recherche Technologique Matériaux, Métallurgie, Procédés | Hard chromium plating process from trivalent chromium |
| 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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