CN102352521B - Environment-friendly barrel-plating type trivalent chromium plating solution and barrel-plating method thereof - Google Patents
Environment-friendly barrel-plating type trivalent chromium plating solution and barrel-plating method thereof Download PDFInfo
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Abstract
The invention provides an environment-friendly barrel-plating type trivalent chromium plating solution and a barrel-plating method thereof, belonging to the field of a plating process. Aiming at the serious problems of large toxicity, heavy pollution, difficult wastewater treatment and the like due to the existence of hexavalent chromium in the existing barrel-plating process for plating chromium, the invention develops an environment-friendly trivalent chromium plating solution suitable for barrel-plating application and a barrel-plating method thereof. The plating solution is mainly prepared from a main salt, a complexing agent, a stabilizing agent, a wetting agent, a conducting salt, a buffering agent and water and also comprises a displacement agent. The invention has the advantages of cleanness and no pollution, and a plating layer has uniform and bright appearance and high corrosion resistance; and in the process provided by the invention, the acidity control is moderate, so that the phenomenon of dissolution of the plating layer can not appear even if the power is switched off. After the displacement agent is introduced into the environment-friendly trivalent chromium plating solution provided by the invention, the displacement and dispersion capabilities of the plating layer can be effectively improved, and the current efficiency and the rate of finished products can be effectively improved. The plating solution is suitable for barrel-plating operation of trivalent chromium on a workpiece.
Description
Invention field
The present invention relates to a kind of electroplating technology, in particular, relate to a kind of barrel plating type trivalent chromium plating technique.
Background technology
Chromium coating has good hardness, wear resistance, solidity to corrosion and ornamental, is one of most widely used plating of electroplating industry.But what electrodeposited chromium mainly adopted at present is rack plating process, extremely rare in barrel plating application, so just limit the application of chrome-plated process in finding plating.Studying carefully its major cause is because chrome-plated process walks, dispersive ability is poor, often there will be low district and plates situation about not covering.Simply electroplate without the part in low district even if traditional barrel plating technique also can only be used for some, particularly easily occur coating acid dissolve during power-off.The corrosion resistance of coating obtained is poor, coating is partially black, and overall cost is very high.
And barrel plating technique contains sexavalent chrome, there are the serious problems such as toxicity is large, pollution is heavy, wastewater treatment is difficult.The existence of the problems referred to above forces chromium barrel plating technique cannot obtain good promotion and application always.
Therefore, the environmental protection trivalent chromium plating technique developing a kind of applicable barrel plating application has just just been of great significance.
Summary of the invention
For the problems referred to above, the invention provides a kind of environmental protection barrel plating type trivalent chromium plating solution and method of barrel electroplating thereof.
First object of the present invention, be to provide a kind of environmental protection barrel plating type trivalent chromium plating solution, this electroplate liquid cleanliness without any pollution in electroplating process, has splendid dispersive ability.
In order to realize first object of the present invention, the invention provides a kind of environmental protection barrel plating type trivalent chromium plating solution, this electroplate liquid, primarily of main salt, complexing agent, stablizer, wetting agent, conducting salt, buffer reagent and water composition, also includes the agent that walks, described main salt is at least one in chromium sulphate or potassium chromium sulfate, described complexing agent is formic acid, at least one in acetic acid and tribromoacetic acid and salt thereof, described stablizer is Padil, mercaptosuccinic acid sodium, at least one in sodium sorbate and sodium hypophosphite, described wetting agent is alkylphenol polyoxyethylene, at least one in hexadecyl diethanolamine Soxylat A 25-7, the described agent that walks is acrylate homopolymer sodium salt, sodium vinyl sulfonate, thiourea derivative and containing at least one in C=S heterogeneous ring compound, described buffer reagent is boric acid, Sodium Tetraborate, at least one in sodium phosphate and Trisodium Citrate, described conducting salt is potassium sulfate, sodium sulfate, at least one in ammonium sulfate.
The present invention also can do following improvement:
The described agent content that walks is 1g/L ~ 120g/L; In the described agent that walks, C=S heterogeneous ring compound is α-thiophene derivant.
Described conducting salt content is 100g/L ~ 200g/L.
Described main salts contg is 10g/L ~ 120g/L.
Described complexing agent content is 1g/L ~ 120g/L.
Described stabiliser content is 1g/L ~ 120g/L.
Described humectant content is 1g/L ~ 8g/L.
Described buffer content is 1g/L ~ 120g/L.
Another object of the present invention is to provide a kind of environmental protection sulfuric acid type trivalent chromium method of barrel electroplating using barrel plating environmental protection barrel plating type trivalent chromium plating solution described in claim 1, uses this method in barrel plating process, current efficiency to be improved significantly.
In order to realize second object of the present invention, a kind of environmental protection sulfuric acid type trivalent chromium method of barrel electroplating provided by the invention, comprises the following steps:
(1) by workpiece pickling and washing;
(2) barrel plating is carried out with above-mentioned a kind of environmental protection barrel plating type trivalent chromium plating solution, condition is: temperature is 40-60 DEG C, cathode current density is 0.1-15ASD, pH value is 3-6, barrel plating time 1-30 minute, the rotating speed of cylinder is 0.5-10 rev/min, and the anode of use is DSA (Dimensionally Stable Anode) iridium titanium coating anode;
(3) with water, plating piece is cleaned up, then dry up.
The present invention also can do following improvement:
In step (2), barrel plating condition is: temperature is 45-55 DEG C, barrel plating cathode current density is 2-5ASD (average current density), rack plating barrel plating current density is 6-15, pH value is 4-5, barrel plating time 20-30 minute, and the rotating speed of cylinder is 1-5 rev/min.
Compared with prior art, the beneficial effect that the present invention has is:
1) adopt a kind of environmental protection barrel plating type trivalent chromium plating solution of the present invention and method of barrel electroplating thereof, cleanliness without any pollution, Deposit appearance is evenly bright, and solidity to corrosion at least doubles than conventional barrel plating chromium;
2) a kind of environmental protection sulfuric acid type trivalent chromium method of barrel electroplating of the present invention, not fluorine-containing silicic acid, its technique acidity control is moderate, even if having a power failure also there will not be coating dissolution phenomena;
3) known by embodiment, after a kind of environmental protection barrel plating type trivalent chromium plating solution of the present invention introduces the agent that walks, effectively can improve coating and walk and dispersive ability;
4) a kind of environmental protection sulfuric acid type trivalent chromium method of barrel electroplating of the present invention effectively can improve current efficiency, reaches about 30%, improves yield rate 80-90% simultaneously, is applicable to barrel plating trivalent chromium on workpiece.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, but any limitation of the invention do not formed.
Following condition is adopted to carry out barrel plating experiment (plating thickness and solidity to corrosion test): coating bath is cylinder chrome-plating bath, cylinder sizes 6 inches × 8 inches (can fill product 1000 grams-2000 grams); Electroplating objects is nickel plating irony hexagonal head bolt, and nickel plating layer thick is 3 μm; PH value is 5; Drum rotational speed is 2rpm; Electroplating time is 30min; Electroplating temperature is 50 DEG C; Current density is 3ASD; Anode is DSA iridium titanium coating anode.
Following condition is adopted to carry out Hull groove experiment (dispersive ability test): coating bath is 267ml Hull groove; Electroplating objects is 10cm × 6cm nickel plating copper sheet, and nickel plating layer thick is 5 μm; PH value is 5; Electroplating time is 5min; Electroplating temperature is 50 DEG C; Current density is 10ASD; Sun level is DSA iridium titanium coating anode; Pre-treatment is through chlorohydric acid pickling and washing.
Experiment obtains sample and tests according to following project and method:
1. outward appearance: range estimation.
2. plating thickness: with the same position (the compromise position in Qu Gao district and low district) of thickness tester test plating back nut.
3. solidity to corrosion test: carry out neutral salt spray test test according to national standard GB/T 10125-1997.
4. dispersive ability test:
δ
1for 1cm place, distance Gao Qu edge thickness, δ
2for for apart from 1cm place, edge, low district thickness.
Comparative example 1
Electroplating bath components:
Chromic anhydride: 320-350g/L
Silicofluoric acid: 4.5-5g/L
Sulfuric acid: 0.5-0.6g/L
Surplus is water
Comparative example 2
Electroplating bath components:
Potassium sulfate: 140g/L
Potassium chromium sulfate: 70g/L
Formic acid: 8g/L
Xitix: 30g/L
Glycerol: 2g/L
Boric acid: 60g/L
Surplus is water
Embodiment 1
Electroplating bath components:
Potassium sulfate: 140g/L
Potassium chromium sulfate: 70g/L
Formic acid/acetic acid/tribromoacetic acid (1: 1: 1): 8g/L
Padil: 30g/L
Alkylphenol polyoxyethylene: 2g/L
Acrylate homopolymer sodium salt: 8g/L
Boric acid: 60g/L
Surplus is water
Embodiment 2
Electroplating bath components:
Potassium sulfate: 140g/L
Potassium chromium sulfate: 70g/L
Formic acid/acetic acid/tribromoacetic acid (1: 1: 1): 8g/L
Padil: 30g/L
Alkylphenol polyoxyethylene: 2g/L
Thiourea derivative: 8g/L
Boric acid: 60g/L
Surplus is water
Embodiment 3
Electroplating bath components:
Potassium sulfate: 140g/L
Potassium chromium sulfate: 70g/L
Formic acid/acetic acid/tribromoacetic acid (1: 1: 1): 8g/L
Padil: 30g/L
Alkylphenol polyoxyethylene: 2g/L
α-thiophene derivant: 8g/L
Boric acid: 60g/L
Surplus is water
Embodiment 4
Electroplating bath components:
Potassium sulfate: 140g/L
Potassium chromium sulfate: 70g/L
Formic acid/acetic acid/tribromoacetic acid (1: 1: 1): 8g/L
Mercaptosuccinic acid sodium: 30g/L
Hexadecyl diethanolamine Soxylat A 25-7: 2g/L
Acrylate homopolymer sodium salt: 8g/L
Boric acid: 60g/L
Surplus is water
Embodiment 5
Electroplating bath components:
Potassium sulfate: 140g/L
Potassium chromium sulfate: 70g/L
Formic acid/acetic acid/tribromoacetic acid (1: 1: 1): 8g/L
Mercaptosuccinic acid sodium: 30g/L
Hexadecyl diethanolamine Soxylat A 25-7: 2g/L
Thiourea derivative: 8g/L
Boric acid: 60g/L
Surplus is water
Embodiment 6
Electroplating bath components:
Potassium sulfate: 140g/L
Potassium chromium sulfate: 70g/L
Formic acid/acetic acid/tribromoacetic acid (1: 1: 1): 8g/L
Mercaptosuccinic acid sodium: 30g/L
Hexadecyl diethanolamine Soxylat A 25-7: 2g/L
α-thiophene derivant: 8g/L
Boric acid: 60g/L
Surplus is water
Embodiment 7
Electroplating bath components:
Potassium sulfate: 140g/L
Potassium chromium sulfate: 70g/L
Formic acid/acetic acid/tribromoacetic acid (1: 1: 1): 8g/L
Padil: 30g/L
Hexadecyl diethanolamine Soxylat A 25-7: 2g/L
α-thiophene derivant: 8g/L
Boric acid: 60g/L
Surplus is water
Embodiment 8
Electroplating bath components:
Potassium sulfate: 140g/L
Potassium chromium sulfate: 70g/L
Formic acid/acetic acid/tribromoacetic acid (1: 1: 1): 8g/L
Mercaptosuccinic acid sodium: 30g/L
Alkylphenol polyoxyethylene: 2g/L
α-thiophene derivant: 8g/L
Boric acid: 60g/L
Surplus is water
Embodiment 9
Electroplating bath components:
Sodium sulfate: 250g/L
Chromium sulphate: 40g/L
Formic acid: 5g/L
Sodium sorbate: 10g/L
Alkylphenol polyoxyethylene: 1g/L
Sodium vinyl sulfonate: 5g/L
Sodium Tetraborate: 50g/L
Surplus is water
Embodiment 10
Electroplating bath components:
Ammonium sulfate: 350g/L
Potassium chromium sulfate: 70g/L
Acetic acid: 20g/L
Sodium hypophosphite: 50g/L
Hexadecyl diethanolamine Soxylat A 25-7: 5g/L
Acrylate homopolymer sodium salt: 12g/L
Sodium phosphate: 80g/L
Surplus is water
Embodiment 11
Electroplating bath components:
Sodium sulfate: 100g/L
Chromium sulphate: 10g/L
Formic acid: 1g/L
Sodium sorbate: 10g/L
Alkylphenol polyoxyethylene: 1g/L
Sodium vinyl sulfonate: 1g/L
Sodium Tetraborate: 1g/L
Surplus is water
Embodiment 12
Electroplating bath components:
Ammonium sulfate: 200g/L
Potassium chromium sulfate: 120g/L
Acetic acid: 120g/L
Sodium hypophosphite: 10g/L
Hexadecyl diethanolamine Soxylat A 25-7: 8g/L
Acrylate homopolymer sodium salt: 120g/L
Sodium phosphate: 120g/L
Surplus is water
Embodiment 13
The electroplate liquid identical with embodiment 3 is adopted to carry out barrel plating, pre-treatment with through chlorohydric acid pickling and washing after, barrel plating condition: temperature is 40, cathode current density is 0.1ASD, pH value is 3,1 minute barrel plating time, the rotating speed of cylinder is 10 revs/min, the DSA iridium titanium coating anode of use;
Embodiment 14
The electroplate liquid identical with embodiment 3 is adopted to carry out barrel plating, pre-treatment with through chlorohydric acid pickling and washing after, barrel plating condition: temperature is 60, cathode current density is 15ASD, pH value is 6,30 minutes barrel plating time, the rotating speed of cylinder is 0.5 rev/min, uses DSA iridium titanium coating anode;
Table 1. table with test results
Comparative example 1 is barrel plating hexavalent chromium plating liquid, and comparative example 2 is conventional sulfuric acid type trivalent chromium plating solution.Electroplate liquid of the present invention is compared with barrel plating sexavalent chrome technique and conventional sulfuric acid type trivalent chromium plating respectively.
From above-mentioned test result, embodiment 1-12 is different due to the additive adopted, and its bright appearance, evenly, can reach the chromic effect of barrel plating, and comparative example 2 outward appearance does not secretly cover in bright, low district.Embodiment 1-12 plating solution contains the agent that walks, and the plating solution of comparative example 1 and 2 is not containing the agent that walks, and the negative electrode of embodiment 1-12 light district and dispersive ability (slotted vane) reach 90% or more, are up to 95%; Much larger than 80% of 70% and the comparative example 2 of comparative example 1; The dispersive ability (slotted vane) of embodiment 1-12 reaches 35% or more, is up to 40%, much larger than 20% of comparative example 1 and comparative example 2.This illustrates that the present invention is by adding the agent that walks in the plating solution, and what can significantly improve plating solution walks capability and dispersive ability.Due to the difference of adopted complexing agent and wetting agent, the current efficiency of embodiment 1-12 reaches 30%-40%, be greater than 18% of 16% and the comparative example 2 of comparative example 1, due to the raising of current efficiency, the thickness of corresponding coating and solidity to corrosion there has also been very large raising, such as, the screw solidity to corrosion (NSST) of embodiment 1-12 reaches as high as 18 hours, be greater than 8 hours of comparative example 1 and the 6h of comparative example 2, this illustrates that the present invention is by adopting different solution composition, significantly improves layers of chrome resistance to corrosion.Simultaneously because the raising of capability and current efficiency walked by coating, the yield rate scope of product is 80%-90%, and the yield rate of comparative example 1 and 2 is only 30% and 40%, makes barrel plating trivalent chromium become possibility.
Simultaneously from above-mentioned test result, adopt the different parameters condition of method of barrel electroplating of the present invention, as embodiment 13 and 14, its bright appearance, even, also can reach the chromic effect of barrel plating.Negative electrode light district and dispersive ability (slotted vane) reach 90%; Much larger than 80% of 70% and the comparative example 2 of comparative example 1; Dispersive ability (slotted vane) reaches 35% or more, much larger than 20% of comparative example 1 and comparative example 2.Its current efficiency reaches more than 30%-, be greater than 18% of 16% and the comparative example 2 of comparative example 1, due to the raising of current efficiency, the thickness of corresponding coating and solidity to corrosion there has also been very large raising, its screw solidity to corrosion (NSST) reaches as high as 18 hours, is greater than 8 hours of comparative example 1 and the 6h of comparative example 2.Simultaneously because the raising of capability and current efficiency walked by coating, the yield rate scope of product is 85%-90%, and the yield rate of comparative example 1 and 2 is only 30% and 40%, makes barrel plating trivalent chromium become possibility.This illustrates within the scope of Parameter Conditions, adopts this method of barrel electroplating to meet the demands.
In sum, a kind of sulfuric acid type barrel plating trivalent chromium plating solution provided by the invention and electro-plating method thereof, have outward appearance brilliant white, covering power be strong, erosion resistance is good, advantage that yield rate is high.
The above embodiments are only the preferred embodiments of the present invention, can not limit interest field of the present invention with this, and therefore, the equivalent variations done according to the present patent application the scope of the claims, still belongs to the scope that the present invention is contained.
Claims (7)
1. an environmental protection barrel plating type trivalent chromium plating solution, primarily of main salt, complexing agent, stablizer, wetting agent, conducting salt, buffer reagent and water composition, is characterized in that: also include the agent that walks, described main salt is at least one in chromium sulphate or potassium chromium sulfate, described complexing agent is formic acid, at least one in acetic acid and tribromoacetic acid and salt thereof, described stablizer is Padil, mercaptosuccinic acid sodium, at least one in sodium sorbate and sodium hypophosphite, described wetting agent is alkylphenol polyoxyethylene, at least one in hexadecyl diethanolamine Soxylat A 25-7, the described agent that walks is acrylate homopolymer sodium salt, sodium vinyl sulfonate, thiourea derivative and containing at least one in C=S heterogeneous ring compound, described buffer reagent is boric acid, Sodium Tetraborate, at least one in sodium phosphate and Trisodium Citrate, described conducting salt is potassium sulfate, sodium sulfate, at least one in ammonium sulfate,
Wherein, described complexing agent content is 1g/L ~ 120g/L, and described stabiliser content is 1g/L ~ 120g/L, and described humectant content is 1g/L ~ 8g/L.
2. a kind of environmental protection barrel plating type trivalent chromium plating solution according to claim 1, is characterized in that: described in the agent content that walks be 1g/L ~ 120g/L.
3. a kind of environmental protection barrel plating type trivalent chromium plating solution according to claim 1, is characterized in that: described conducting salt content is 100g/L ~ 200g/L.
4. a kind of environmental protection barrel plating type trivalent chromium plating solution according to claim 1, is characterized in that: described main salts contg is l0g/L ~ 120g/L.
5. a kind of environmental protection barrel plating type trivalent chromium plating solution according to claim 1, is characterized in that: described buffer content is 1g/L ~ 120g/L.
6. an environmental protection barrel plating type trivalent chromium method of barrel electroplating, is characterized in that comprising the following steps:
(1) by workpiece pickling and washing;
(2) barrel plating is carried out with environmental protection barrel plating type trivalent chromium plating solution a kind of described in any one of claim 1-5, condition is: temperature is 40-60 DEG C, cathode current density is 0.1-15ASD, pH value is 3-6, barrel plating time 1-30 minute, the rotating speed of cylinder is 0.5-10 rev/min, and the anode of use is DSA(Dimensionally Stable Anode) iridium titanium coating anode;
(3) with water, plating piece is cleaned up, then dry up.
7. a kind of environmental protection barrel plating type trivalent chromium method of barrel electroplating according to claim 6, it is characterized in that: in step (2), barrel plating condition is: temperature is 45-55 DEG C, barrel plating cathode current density is 2-5ASD, rack plating barrel plating current density is 6-15, pH value is 4-5, barrel plating time 20-30 minute, the rotating speed of cylinder is 1-5 rev/min.
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| TWM440877U (en) * | 2012-04-20 | 2012-11-11 | Universal Trim Supply Co Ltd | Workpiece containing glossy cladding layer |
| CN103510096A (en) * | 2012-06-20 | 2014-01-15 | 江苏华宇印涂设备集团有限公司 | Oil transmission roller |
| CN103334149B (en) * | 2013-06-13 | 2016-04-27 | 中国科学院过程工程研究所 | A kind of cycle intermittent type rolls hard chromium plating device and using method |
| CN103526245A (en) * | 2013-09-30 | 2014-01-22 | 朱卓敏 | New environment-friendly process for chromium barrel plating after chloride zinc plating |
| CN105018973A (en) * | 2014-11-27 | 2015-11-04 | 太仓市金鹿电镀有限公司 | Environment-friendly electroplating liquid and electroplating process |
| 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 |
| CN104789996A (en) * | 2015-04-15 | 2015-07-22 | 吉林莱德化学科技有限公司 | Trivalent chrominm plating electroplating liquid |
| CN107313078A (en) * | 2016-04-27 | 2017-11-03 | 中国科学院金属研究所 | A kind of trivalent chromium plating solution and preparation method thereof |
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| US3917517A (en) * | 1973-10-10 | 1975-11-04 | Int Lead Zinc Res | Chromium plating electrolyte and method |
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