CN108677181B - Additive for mechanical deposition of cadmium - Google Patents
Additive for mechanical deposition of cadmium Download PDFInfo
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- CN108677181B CN108677181B CN201810453406.3A CN201810453406A CN108677181B CN 108677181 B CN108677181 B CN 108677181B CN 201810453406 A CN201810453406 A CN 201810453406A CN 108677181 B CN108677181 B CN 108677181B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
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Abstract
本发明公开一种机械沉积镉用添加剂，属于金属表面防护技术领域。本发明所述添加剂的组分及质量百分比为：丁炔二醇1%~3%，乳化剂OP‑10 1.5%~4%，柠檬酸6%~10%，木质素磺酸钠3%~5%，苹果糖酸钠0.5%~2%，硫酸镉3~10%，氯化亚锡10~18%、余量为水。施镀时，本发明添加剂的组分能够保证基体和镉粉表面处于清洁状态，控制镉粉具有合适的团聚尺寸，对金属离子产生较强的吸附、螯合作用，能够实现较短时间内（3～5min）获得10μm厚度的镀层沉积。The invention discloses an additive for mechanical deposition of cadmium, which belongs to the technical field of metal surface protection. The components and mass percentages of the additive of the present invention are: butynediol 1%~3%, emulsifier OP-10 1.5%~4%, citric acid 6%~10%, sodium lignosulfonate 3%~ 5%, sodium malate 0.5%~2%, cadmium sulfate 3~10%, stannous chloride 10~18%, and the balance is water. When plating, the components of the additive of the present invention can ensure that the substrate and the surface of the cadmium powder are in a clean state, control the cadmium powder to have a suitable agglomeration size, produce strong adsorption and chelation for metal ions, and can achieve a relatively short period of time ( 3 to 5 min) to obtain a coating deposition with a thickness of 10 μm.
Description
Technical Field
The invention relates to an additive for mechanically depositing cadmium, belongs to the technical field of metal surface treatment, is used for mechanical deposition of a cadmium coating on the surface of a steel part, and specifically belongs to the technical field of metal coating on a steel substrate.
Background
Cadmium plating has potential environmental pollution, and the plating layer is easy to have hydrogen embrittlement and cadmium embrittlement, but because the cadmium plating has the excellent marine environment corrosion resistance, the cadmium plating is still the main protective measure of steel-based parts for marine equipment at present, and is particularly applied to surface protection of fasteners, connecting pieces and the like of ship equipment, and the cadmium plating is still the main first choice; the current cadmium plating process is basically carried out by adopting a cadmium plating process, and the cadmium plating of high-strength steel bolts and connecting pieces such as 300M, 30CrMnSiNi2A, A-100 and the like is easy to have hydrogen brittleness and cadmium brittleness, so that the fatigue life of a base material is seriously influenced.
Compared with the traditional electroplating and hot-dip plating, the mechanical deposition plating has the advantages of operation at room temperature, no hydrogen embrittlement after plating, easy control of plating thickness, no cadmium ion diffusion, no tempering softening and the like; the mechanical deposition plating process has no electrolytic effect and high temperature metallurgical reaction; therefore, the mechanical deposition plating process has no electrolytic hydrogen evolution and no corrosion of high temperature molten metal. Therefore, the cadmium plating layer prepared by the mechanical deposition method has obvious advantages in view of the reasons of hydrogen embrittlement and cadmium embrittlement. However, metal cadmium is different from metal zinc, zinc belongs to sacrificial anode protection on steel substrates, and electrode potential of cadmium is more positive than that of iron, so cadmium belongs to a cathode protection coating on the steel substrates. Because of the difference of the potentials of the zinc electrode and the cadmium electrode and the difference of the potential sequencing positions of the zinc electrode, the traditional zinc mechanical deposition principle and the activator for mechanical zinc deposition cannot be applied to the mechanical deposition process for moving to cadmium. Tests show that when the cadmium is plated by adopting a mechanical zinc deposition process, the deposition speed of cadmium powder is low, the thickness of a plating layer is not increased to 10 mu m after the cadmium powder is added for 10 minutes, the deposition process is unstable, the effective utilization rate of the cadmium powder is lower than 50 percent, and the plating layer with the expected thickness is difficult to obtain. The literature search at home and abroad shows that the related researches on the aspects of the mechanical cadmium deposition process flow, the additive, the process principle and the like are few. In view of the above, the development of the rapid mechanical deposition research of the cadmium plating layer has important practical significance for many problems existing in the traditional cadmium electroplating, which is also a problem to be solved by technologists in the technical field of metal surface treatment.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provides an additive for mechanical deposition of cadmium, which is used for realizing rapid mechanical deposition of cadmium on the surface of a steel part and comprises the following components in percentage by mass: 1-3% of butynediol, 101.5-4% of emulsifier OP-101, 6-10% of citric acid, 3-5% of sodium lignosulfonate, 0.5-2% of sodium malate, 3-10% of cadmium sulfate, 10-18% of stannous chloride and the balance of water, wherein the sum of the mass percentages of all the components is 100%.
The components of the additive for mechanically depositing cadmium are industrial chemical raw materials.
The invention relates to a preparation method of an additive for mechanically depositing cadmium, which comprises the following steps: firstly, adding water and citric acid into a container, then adding butynediol, an emulsifier OP-10, sodium lignosulfonate, sodium malate, cadmium sulfate and stannous chloride, and uniformly stirring to obtain an additive aqueous solution.
When the additive for mechanically depositing cadmium is used, the addition quantity Q of the activator is as follows when the thickness of a plating layer is increased by 10 mu m:
q: the addition amount is unit ml;
s: surface area of plated part, unit m2；
40-45: the coefficient is selected from 40 to 45 according to the flatness of the surface of the plated part.
The process steps of the additive for mechanically depositing cadmium in the invention when in use are as follows:
(1) pretreatment: the degreasing and degreasing methods commonly used in the electroplating, hot dipping and mechanical plating processes, such as a hot alkali method, an ultrasonic method, an oxidation method and the like, are adopted to remove grease on the surface of the workpiece, the rust removal methods commonly used in the electroplating, hot dipping and mechanical plating processes, such as a chemical pickling method, a sand blasting shot blasting method and the like, are adopted to remove rust on the surface of the workpiece, and the surface of the pretreated steel workpiece is exposed to a clean metal surface layer.
(2) Establishing a Cd-Sn base layer: the method is similar to a mechanical galvanizing method, uses general mechanical plating equipment, and establishes a Cd-Sn base layer on the surface of a steel part by adding cadmium powder and stannous sulfate into a roller of the mechanical plating equipment.
(3) And (4) cadmium plating: cadmium powder is added into the drum, then the additive aqueous solution is measured and added according to the surface area of the plated part, and the drum rotates for 3-5 minutes (the cadmium powder and the additive aqueous solution can be added in a plurality of times of circulation according to the required thickness of the cadmium layer in the process, and the time interval of the circulation feeding is 3-5 minutes).
(4) And (3) post-treatment: when the thickness of the plating layer is reached, unloading and separating, drying the plated piece at the temperature of not higher than 120 ℃, and obtaining a bright silvery-white cadmium plating layer on the surface of the steel piece.
The invention has the beneficial effects that:
(1) the rapid deposition of cadmium powder is realized, and the plating layer is thickened rapidly.
When the additive for mechanically depositing cadmium is added into the plating cylinder, components in the additive act on the surface of a matrix, the surface of cadmium powder particles can be ensured to be always in a clean state, meanwhile, the plating solution environment added with the additive promotes the potential negative shift of the surface of the cadmium powder particles, the adsorption and deposition of the cadmium powder are accelerated, the plating layer deposition with the thickness of 10 microns can be obtained within a short time (3-5 min), and the thickening speed is obviously higher than that of cadmium plated by a mechanically deposited zinc activator (the thickening speed of the plating layer is less than 10 microns in 10 min).
(2) The stable deposition of cadmium powder is realized, and the plating layer is thickened uniformly.
After the additive for rapid mechanical deposition of cadmium is added into the plating cylinder, the additive is dissolved in the plating solution, so that the cadmium powder can be controlled to have a proper agglomeration size, the cadmium powder or cadmium powder clusters can be continuously and uniformly adsorbed and deposited on the surface of a substrate, and the plating layer can be uniformly thickened in each feeding period.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the scope of the present invention is not limited to the examples.
The raw materials used in the embodiment of the invention are industrial chemical raw materials, and the water is clean tap water.
The preparation method of the additive for mechanically depositing cadmium in the embodiments 1-4 of the invention comprises the following steps: the raw materials are respectively weighed according to the mass percentage, firstly, water and citric acid are added into a container, then butynediol, an emulsifier OP-10, sodium lignosulfonate and sodium malate are added, finally, cadmium sulfate and stannous chloride are added, and the mixture is uniformly stirred to obtain the aqueous solution of the additive.
Example 1
The additive for rapid mechanical deposition of cadmium comprises the following components in percentage by mass: 1% of butynediol, an emulsifier OP-104%, 10% of citric acid, 3% of sodium lignosulfonate, 0.5% of sodium malate, 3% of cadmium sulfate, 18% of stannous chloride and 60.5% of water.
The additive for rapid mechanical deposition of cadmium is used for mechanical deposition of cadmium coatings on surfaces of steel workpieces, wherein the workpiece to be coated is 200kg of a standard flat gasket with the diameter of phi 24mm and the thickness of 3.0 mm, the surface area to be coated is about 17 square meters, and the coating thickness is required to be 10 micrometers. During plating, a cadmium-tin base layer is built on the pretreated gasket, 1360g of cadmium powder is added into the plating cylinder, 680ml of prepared additive aqueous solution is added into the plating cylinder, and the plating cylinder continues to rotate for 5 minutes; then unloading and separating are carried out, and a bright silvery-white cadmium coating is obtained on the surface of the gasket. The plating layer still presents bright silvery white after being dried at 120 ℃ for +30min, the thickness of the cadmium plating layer is about 11 mu m through cross section metallographic method observation, and the plating layer thickness is uniform.
Comparative example of the present embodiment: the workpiece to be plated is 200kg of standard flat gasket with the diameter of 24mm and the thickness of 3.0 mm, the surface area to be plated is about 17 square meters, and the thickness of the plating layer is required to be 10 mu m. During plating, a cadmium-tin base layer is built on the pretreated gasket, 800ml of mechanical zinc plating retention activator (commercially available, addition amount and use method reference, mechanical zinc plating technology foundation, mechanical industry publisher, 2013, page 194) is added into a plating cylinder, 1360g of cadmium powder is added into the plating cylinder, 1224ml of mechanical zinc plating deposition activator (commercially available, addition amount and use method reference, mechanical zinc plating technology foundation, mechanical industry publisher, 2013, page 195) is added into the plating cylinder, the plating cylinder continues to rotate for 5 minutes, and the surface of the gasket is sampled and observed to be a gray and loose cadmium layer; and (4) continuously rotating the plating barrel for 5 minutes, then unloading and separating, and obtaining a silvery white cadmium plating layer on the surface of the gasket. The coating still presents silvery white after being dried at 120 ℃ for +30min, the thickness of the cadmium coating is about 6 mu m when the cross section metallographic method is used for observing, and the thickness of the coating is not uniform.
The comparison shows that after the additive for cadmium is rapidly and mechanically deposited by the method, the cadmium powder deposition speed is high, the plating layer is thickened quickly, and the effective utilization rate of the cadmium powder is high.
Example 2
The additive for rapid mechanical deposition of cadmium comprises the following components in percentage by mass: 3% of butynediol, an emulsifier OP-102%, 6% of citric acid, 5% of sodium lignosulfonate, 2% of sodium malate, 10% of cadmium sulfate, 12% of stannous chloride and 10% of water.
The additive for rapid mechanical deposition of cadmium is used for mechanical deposition of cadmium plating on the surface of a steel workpiece, the workpiece to be plated is 200kg of an 8.8-grade standard bolt of M16, the surface area to be plated is 8.6 square meters, and the plating thickness is required to be 20 micrometers. During plating, a cadmium-tin base layer is built on the pretreated bolt, 688g of cadmium powder is added into a plating barrel, 800ml of prepared additive aqueous solution is added into the plating barrel, and the plating barrel continues to rotate for 4 minutes; 688g of cadmium powder and 800ml of aqueous solution of an activating agent are added into the plating barrel again, the plating barrel continues to rotate for 6 minutes, then the materials are discharged and separated, and a bright silvery-white cadmium plating layer is obtained on the surface of the bolt. The plating layer still presents bright silvery white after being dried at 110 ℃ for +30 min. The thicknesses of the coatings at five points on the plane of the bolt head detected by a magnetic measurement method are respectively 23 micrometers, 21 micrometers, 26 micrometers, 19 micrometers and 24 micrometers; and testing the mechanical properties of the bolt to be qualified through a post-plating tensile test.
Comparative example of the present embodiment: the workpiece to be plated is 200kg of 8.8-grade standard bolt of M16, the surface area to be plated is 8.6 square meters, and the thickness of the plated layer is required to be 20 mu M. During plating, a cadmium-tin base layer is built on the pretreated gasket, then 688ml of mechanical galvanizing retention activator (commercially available, additive amount and use method reference, mechanical galvanizing technology foundation, mechanical industry publisher, 2013, page 194) is added into a plating cylinder, 688g of cadmium powder is added into the plating cylinder, then 620ml of mechanical galvanizing deposition activator (commercially available, additive amount and use method reference, mechanical galvanizing technology foundation, mechanical industry publisher, 2013, page 195) is added into the plating cylinder, the plating cylinder continues to rotate for 5 minutes, the surface of the gasket is observed by sampling, the surface of the gasket is a gray and loose cadmium layer, and the plating cylinder continues to rotate for 5 minutes; 688g of cadmium powder and 620ml of mechanical galvanizing B additive are added into the plating barrel again, the plating barrel continues to rotate for 10 minutes, then the materials are discharged and separated, a semi-bright cadmium plating layer is obtained on the surface of the bolt, and the cadmium powder in the wastewater after separation is obvious in residue. The plating layer still presents semi-bright color after being dried at 110 ℃ for 30 min. The thicknesses of the coatings at five points of the plane of the bolt head detected by a magnetic measurement method are respectively 13 microns, 9 microns, 19 microns, 15 microns and 13 microns; the thickness of the plating layer is not uniform.
The comparison shows that after the additive for cadmium is rapidly and mechanically deposited by the method, the cadmium powder deposition speed is high, the plating layer is thickened quickly, and the effective utilization rate of the cadmium powder is high.
Example 3
The additive for rapid mechanical deposition of cadmium comprises the following components in percentage by mass: 2% of butynediol, 101.5% of emulsifier OP-8%, 8% of citric acid, 4% of sodium lignosulfonate, 1% of sodium malate, 5% of cadmium sulfate, 10% of stannous chloride and 68.5% of water.
The additive for rapid mechanical deposition of cadmium is used for mechanical deposition of cadmium coatings on surfaces of steel workpieces, wherein the workpiece to be coated is 200kg of a standard flat gasket with the diameter of phi 20mm and the thickness of 3.0 mm, the surface area to be coated is about 21 square meters, and the coating thickness is required to be 10 micrometers. During plating, a cadmium-tin base layer is built on the pretreated gasket, then 840g of cadmium powder is added into the plating cylinder, 470ml of prepared additive aqueous solution is added into the plating cylinder, and the plating cylinder continues to rotate for 4 minutes; adding 840g of cadmium powder and 470ml of additive aqueous solution into the plating cylinder again, and continuing to rotate the plating cylinder for 6 minutes; then unloading and separating are carried out, and a bright silvery-white cadmium coating is obtained on the surface of the gasket. The plating layer still presents bright silvery white after being dried at 110 ℃ for +50 min. The thickness of the coating on the surface of the gasket was measured to be about 21 μm by magnetic measurement.
Comparative example of the present embodiment: the workpiece to be plated is 200kg of standard flat gasket with the diameter of 20mm and the thickness of 3.0 mm, the surface area to be plated is about 21 square meters, and the thickness of the plating layer is required to be 10 mu m. During plating, a cadmium-tin base layer is built on the pretreated gasket, 840g of cadmium powder is added into a plating cylinder, 800ml of mechanical plating retention activator (a mechanical plating technical basis, a mechanical industry publisher, 2013, page 194) is added into the plating cylinder, 840g of cadmium powder is added into the plating cylinder, 756ml of mechanical plating deposition activator (a mechanical plating technical basis, a mechanical industry publisher, 2013, page 195) is added into the plating cylinder, the plating cylinder continues to rotate for 5 minutes, then unloading and separation are carried out, a gray cadmium plating layer is obtained on the surface of the gasket, and more cadmium powder remains in waste water after separation. The coating still appears gray after being dried at 110 ℃ for +50 min. The thickness of the coating on the surface of the gasket was about 4 μm as measured by magnetic measurements.
The comparison shows that after the additive for cadmium is rapidly and mechanically deposited by the method, the cadmium powder deposition speed is high, the plating layer is thickened quickly, and the effective utilization rate of the cadmium powder is high.
Example 4
The additive for rapid mechanical deposition of cadmium comprises the following components in percentage by mass: 2.5 percent of butynediol, 103 percent of emulsifier OP-103, 8 percent of citric acid, 4.5 percent of sodium lignosulfonate, 1.5 percent of sodium malate, 10 percent of cadmium sulfate, 16 percent of stannous chloride and 54.5 percent of water.
The additive for rapid mechanical deposition of cadmium is used for mechanical deposition of cadmium coatings on surfaces of steel workpieces, the workpiece to be coated is 200kg of a flat plate with a central opening phi of 20mm, wherein the length of the flat plate is 80mm multiplied by 80mm, the width of the flat plate is multiplied by 8mm, the material is Q345, the surface of a matrix is subjected to sand blasting, the surface area to be coated is 8.5 square meters, and the thickness of the coating is required to be 20 micrometers. During plating, a cadmium-tin base layer is built on the pretreated workpiece, 680g of cadmium powder is added into a plating cylinder, 385ml of prepared additive aqueous solution is added into the plating cylinder, and the plating cylinder continues to rotate for 5 minutes; 680g of cadmium powder and 385ml of additive aqueous solution are added into the plating cylinder again, and the plating cylinder continues to rotate for 6 minutes; then unloading and separating are carried out, and a bright silvery-white cadmium coating is obtained on the surface of the workpiece. The coating still presents bright silvery white after being dried at 120 ℃ for +45 min; the thicknesses of the plating layers detected at 5 points on the surface of the workpiece by the magnetic measurement method were 22 μm, 25 μm, 23 μm, 20 μm, and 24 μm, respectively.
Comparative example of the present embodiment: the workpiece to be plated is a flat plate piece 200kg with the central opening diameter phi of 20mm and the material quality of Q345, wherein the length of the workpiece is 80mm multiplied by 8mm, the surface of a matrix is subjected to sand blasting treatment, the surface area to be plated is 8.5 square meters, and the thickness of a plating layer is required to be 20 mu m. During plating, a cadmium-tin base layer is built on a pretreated workpiece, 680ml of mechanical zinc plating retention activator (commercially available, addition amount and use method reference, mechanical zinc plating technology foundation, mechanical industry publisher, 2013, page 194) is added into a plating cylinder, 680g of cadmium powder is added into the plating cylinder, 612ml of mechanical zinc plating deposition activator (commercially available, addition amount and use method reference, mechanical zinc plating technology foundation, mechanical industry publisher, 2013, page 195) is added into the plating cylinder, the plating cylinder continues to rotate for 5 minutes, a sample is taken to observe the surface of the gasket to find that the surface of the gasket is a gray and loose cadmium layer, and the plating cylinder continues to rotate for 5 minutes; and adding 680g of cadmium powder and 612ml of mechanical zinc plating B additive into the plating cylinder again, continuously rotating the plating cylinder for 6 minutes, then unloading and separating, obtaining a gray cadmium plating layer on the surface of the workpiece, and leaving much cadmium powder in the waste water after separation. The coating still appears gray after being dried at 120 ℃ for +45 min. The magnetic measurement method detects that the thickness of the coating on the surface of the workpiece is about 11 mu m and the thickness of the coating is not uniform.
The comparison shows that after the additive for cadmium is rapidly and mechanically deposited by the method, the cadmium powder deposition speed is high, the plating layer is thickened quickly, and the effective utilization rate of the cadmium powder is high.
Claims (1)
1. An additive for mechanically depositing cadmium, comprising: the additive comprises the following components in percentage by mass: 1-3% of butynediol, 101.5-4% of emulsifier OP-101, 6-10% of citric acid, 3-5% of sodium lignosulfonate, 0.5-2% of sodium malate, 3-10% of cadmium sulfate, 10-18% of stannous chloride and the balance of water.
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| US3328197A (en) * | 1965-02-08 | 1967-06-27 | Minnesota Mining & Mfg | Mechanical plating |
| US3479209A (en) * | 1966-07-22 | 1969-11-18 | Peen Plate Inc | Mechanical plating |
| CN101230457B (en) * | 2008-02-22 | 2010-06-02 | 昆明理工大学 | Zinc-Nickel Composite Mechanical Plating Process |
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