CN115787053A - High-stability electroplating additive and preparation method thereof - Google Patents
High-stability electroplating additive and preparation method thereof Download PDFInfo
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- CN115787053A CN115787053A CN202211455891.0A CN202211455891A CN115787053A CN 115787053 A CN115787053 A CN 115787053A CN 202211455891 A CN202211455891 A CN 202211455891A CN 115787053 A CN115787053 A CN 115787053A
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- additive
- electroplating
- stability
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000011737 fluorine Substances 0.000 claims abstract description 24
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Abstract
The invention discloses a high-stability electroplating additive and a preparation method thereof, wherein the additive comprises the following components in percentage by mass: 100-200 parts of blue vitriol, 25-40 parts of sulfuric acid, 40-80 parts of chloride ions, 20-80 parts of a buffering agent, 6-12 parts of a primary brightening agent, 11-44 parts of an emulsifying agent, 20-60 parts of a secondary brightening agent, 20-25 parts of a softening agent, 1-10 parts of an inhibitor, 5-15 parts of a cylinder opener, 1-10 parts of fluorine-containing glycerol ether, 60-100 parts of a carrier brightening agent and 1-10 parts of a microporous nickel additive. The electroplating additive used in the invention has extremely high stability, can not be decomposed in the plating solution, can not generate the phenomena of precipitation, color change and the like after multiple times of electroplating and long-time placement, and ensures the brightness of the PCB and the qualification rate of the PCB after electroplating.
Description
Technical Field
The invention relates to the field of electroplating additives, in particular to a high-stability electroplating additive and a preparation method thereof.
Background
Electroplating is used as a surface processing technology for surface modification, has great flexibility, can apply different coatings on the surface of a material according to different requirements to meet the requirements of different properties, and expands the application range of metal materials, so that electroplating is widely applied to the fields of various industrial production and scientific research. In the mechanical manufacturing industry, electroplating is the main means of corrosion protection and service life extension of metal parts. The loss caused by corrosion is large in the chemical industry, the petroleum industry, coastal areas and damp and hot areas, the plating layer has stronger corrosion resistance in the environment, and the plating process is simple and low in cost, so that the plating has more obvious corrosion resistance in the industries such as the petrochemical industry and the like. In addition to this, this makes the use of electroplating more widespread.
Another advantage of electroplating is that the coating is typically only a thin metal layer, in the range of a few microns to tens of microns, which can result in substantial savings in precious metal materials. Compared with other surface treatment methods, the electroplating process has simple equipment, easy control of operation conditions and great economic significance, so the electroplating process is gradually developed into a manufacturing method for obtaining surface materials. Electroplating is an important form of deposition by which more than half of the periodic table of elements can be deposited. The electroplating process comprises activation, cathode cleaning and upper plating of 2~4. In recent decades, electroplating, which is a process of electrodeposition, in which metal ions (or complex ions) in an electrolyte are reduced to a metal (or alloy) on a cathode surface under the action of direct current, and the metal to be electroplated on a substrate is provided by the metal electrolyzed from an electroplating solution, has been widely used in various industries, resulting in the development of electroplating from a technology of precise science. This requires that the plating must have two conditions: firstly, the plating solution must contain ions to be plated; and the second is to pass direct current. The electroplating device mainly comprises: a direct current power supply; a solution capable of conducting an electric current and having a composition; two electrodes in contact with the plating solution, the plating part is hung on the cathode, and the anode is generally the metal to be covered.
The electroplating process is a method for plating a layer of metal on a conductor by utilizing the electrolysis principle, wherein plating metal or other insoluble materials are used as an anode during electroplating, a workpiece to be plated is used as a cathode, and cations of the plating metal are reduced into a plating layer on the surface of the cathode. By electroplating, the properties of the cathode such as corrosion resistance, strength, hardness, wear resistance, conductivity, heat resistance, etc. can be improved, and the surface can be decoratively beautified. The multilayer electroplating process is to perform several layers of electroplating processes with different materials on the same electroplated product, and the multilayer electroplating can not only reduce the thickness of a coating, but also improve the performance of the coating. Nickel has good physical and chemical properties, can play a role in mechanical protection, has an electrochemical protection function, and can be used as a plating layer for decorative appearance.
For example, chinese patent CN109609979B discloses a multilayer nickel electroplating additive for improving stability, the nickel plating process adopts a smaller current density, reduces energy consumption, and has short electroplating time, good bright effect after nickel plating and high stability.
But compared with other nickel plating systems, such as nickel plating electrolytes of full chloride, sulfamate, citrate, pyrophosphate, fluoroborate and the like, the sulfate nickel plating system is the basis of a plurality of decorative nickel plating processes, and the nickel plating electrolyte has simple composition, cannot reduce the workload brought by workpiece polishing and burnishing, and is not more beneficial to the continuous processing.
An effective solution to the problems in the related art has not been proposed yet.
Disclosure of Invention
Aiming at the problems in the related art, the invention provides a high-stability electroplating additive and a preparation method thereof, so as to overcome the technical problems in the prior related art.
Therefore, the invention adopts the following specific technical scheme:
according to one aspect of the invention, a high-stability electroplating additive is provided, and comprises the following components in percentage by mass:
100-200 parts of copper sulfate pentahydrate;
25-40 parts of sulfuric acid;
40-80 parts of chloride ions;
20-80 parts of a buffering agent;
6-12 parts of a primary brightening agent;
11-44 parts of an emulsifier;
20-60 parts of secondary brightening agent;
20-25 parts of a softening agent;
1-10 parts of an inhibitor;
5-15 parts of a jar opening agent;
1-10 parts of fluorine-containing glycerol ether;
60-100 parts of a carrier brightener;
1-10 parts of a microporous nickel additive.
Further, the buffer includes boric acid, phosphoric acid, citric acid, carbonic acid, acetic acid, and barbituric acid.
Further, the primary brightening agent contains = C-SO 2 -an organic compound of structure.
Further, the emulsifier comprises sodium allyl sulfonate, polyoxyethylene ether and sodium propargyl sulfonate, and the mass fraction ratio is 6:4:1.
further, the secondary brightener includes 1,4-butynediol, diethoxybutynediol, ethoxypropynol, diethylpropynylamine, and propane pyridinium sulfate, and the method of preparing the secondary brightener includes the steps of:
adding 1,4-butynediol, diethoxybutynediol, ethoxypropynyl alcohol, diethylpropynyl amine, and propidium sulfate sequentially into a reactor;
the mixed liquid is stirred by adjusting the number of jet ports below the blades of the reactor and the stirring speed;
the secondary brightener is obtained by adding a proper amount of acid into the reactor and reducing the pH value, and controlling the pH value of the mixed solution to be about 7.
Further, the softening agent comprises ester quaternary ammonium salt, dialkyl quaternary ammonium salt, alkyl acyl quaternary ammonium salt, pyridine quaternary ammonium salt type and imidazole type softening agent.
Further, the cylinder opening agent comprises the following components in percentage by mass of 1:1, an aldehyde compound and a manganese-containing compound;
wherein the aldehyde compounds comprise acetaldehyde propylene glycol acetal, phenylpropargyl aldehyde acetal, and,
-diketone compounds, dimethoxymethane, p-methoxybenzaldehyde, 2-furylaldehyde, 2-methylpropionaldehyde and p-dimethylaminobenzaldehyde;
the manganese-containing compound comprises manganese naphthenate, manganous anhydride, manganese anhydride, basic manganese oxide, manganese carbonate and high manganese anhydride.
Further, the fluorine-containing glycidyl ether comprises perfluorononene polyglycerol ether, octafluorobiphenyl diglycidyl ether and hexadecafluorononyl glycidyl ether.
Further, the carrier brightening agent is a nonionic polyether compound.
According to another aspect of the present invention, there is also provided a method for preparing a high stability type plating additive, the method comprising the steps of:
s1, weighing a proper amount of blue copperas solution, adding the blue copperas solution into deionized water, stirring and dissolving, adding required amount of sulfuric acid and chloride ions, and stirring uniformly to obtain a base solution;
s2, putting the base solution into a reactor, and setting plating conditions of the reactor;
s3, adding a buffering agent, a primary brightening agent, an emulsifying agent and a secondary brightening agent into the base liquid in sequence while stirring, and controlling the stirring speed to be 2000rpm/min;
and S4, regulating and controlling the reaction temperature of the reactor, controlling the temperature at room temperature, sequentially adding a softening agent, an inhibitor, a cylinder opening agent, fluorine-containing glyceryl ether and a carrier brightener, and uniformly stirring to obtain the high-stability electroplating additive.
Boric acid: the crystal is white powder crystal or scale-shaped crystal with triclinic axis, has smooth hand feeling and no odor, is dissolved in water, alcohol, glycerin, ether and essential oil, has weak acidity in water solution, and can be used in glass, enamel, ceramic, medicine, metallurgy, leather, dye, pesticide, fertilizer, textile and other industries.
Sodium alkyl benzene sulfonate: the solid can be dissolved in water, the active matter content is 30-40%, the unsaponifiable matter content is 3% (calculated by 100% active matter), the pH value is about 8, and the solid has the surface activity of decontamination, wetting, foaming, emulsification and dispersion.
Sodium allyl sulfonate: the third monomer of acrylic fiber improves the dyeing property of the fiber, has firm coloring, is used for the nickel electroplating brightener, improves the metal distribution capability and the ductility, and is a water quality treating agent and an oil field drilling mud additive.
Polyoxyethylene ether, also known as polyoxyethylene or polyethylene oxide, is a crystalline, thermoplastic, water-soluble polymer, which is a novel water-soluble resin and is a nonionic surfactant. The demand of various industries for the polyoxyethylene ether is increasing day by day, and the production and application prospects of the polyoxyethylene ether are wide from the development field.
Propargyl sodium sulfonate, electroplate brightener, can improve the brightness of current density area, enhance the ability of walking, level ability, impurity tolerance;
1,4-butynediol: white or light yellow crystal, white rhombic crystal (light yellow after moisture absorption), solubility of the crystal is soluble in water, acid solution, ethanol and acetone, slightly soluble in chloroform and insoluble in benzene and ether, solid butynediol with other properties is easy to deliquesce and toxic in air with 25 ℃, has the chemical property of binary primary alcohol, and can also carry out addition reaction.
Diethoxybutylene glycol: amber viscous liquid like alcohol smell.
The esterquat is a novel cationic surfactant, and has excellent softness, antistatic property and yellowing resistance. Does not contain APEO and formaldehyde, is easy to biodegrade, and is green and environment-friendly. The dosage is less, the effect is good, the preparation is convenient, the comprehensive cost is low, and the cost performance is extremely high. Is the best substitute of dioctadecyl dimethyl ammonium chloride (D1821), film, olein and the like.
Dimethoxymethane: also named as methylene dimethyl ether and methylal, is a colorless liquid, has the smell similar to chloroform, is mainly used as a solvent and an analytical reagent, has irritation to mucous membranes and anesthetic action, and can cause irritation to the nose and the throat due to vapor inhalation; dizziness and the like appear when the medicine is inhaled at high concentration, the damage to eyes can occur, and the damage can be caused by dry skin after long-term skin contact for a plurality of days.
P-methoxybenzaldehyde: is colorless to light yellow liquid at normal temperature, and has smell similar to that of hawthorn. And preparing a main body spice with the hawthorn flower fragrance. Can also be used in lilac, orchid, sunflower, acacia, mimosa, robinia pseudoacacia, magnolia, vanilla, sweet bean flower and other floral essences and newly mown grass, osmunda japonica, aldehyde fragrance and other non-floral essences. It can also be used in heavy wood-flavor essence such as lignum Santali albi. Also used in soap essences. It is used in food to sweeten and harmonize flavor.
P-dimethylamine benzaldehyde: it is used as dye intermediate, and also used as reagent for measuring urobilin, indole, alkaloid, etc. and chromatographic analysis reagent.
Manganese carbonate: is a raw material for manufacturing soft magnetic ferrite of telecommunication equipment, synthesizing manganese dioxide and manufacturing other manganese salts. Used as a catalyst for desulfurization, as a pigment for enamels, paints and varnishes. Also as a fertilizer and feed additive. It can be used for medicine, welding electrode auxiliary material, etc. and can be used as raw material for producing electrolytic manganese metal.
The invention has the beneficial effects that:
1. the invention improves the performance of the plating solution and the plating layer to a great extent by adding the emulsifier, the secondary brightener, the primary brightener, the carrier brightener and the like, and the additive of the invention can not generate impurities in the plating layer, thereby obviously improving the surface brightness of the plating layer and ensuring the uniformity of the plating layer.
2. The nickel plating process containing the multilayer nickel electroplating additive provided by the invention adopts a smaller current density, reduces the energy consumption, and has the advantages of short electroplating time, good bright effect after nickel plating and high stability.
3. The electroplating additive used in the invention has extremely high stability, can not be decomposed in the plating solution, can not generate the phenomena of precipitation, color change and the like after multiple times of electroplating and long-time placement, and ensures the brightness of the PCB and the qualification rate of the PCB after electroplating.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a flow chart of a method for preparing a high stability electroplating additive according to an embodiment of the present invention;
FIG. 2 is a graph comparing the hardness of the PCB boards treated with the plating additives prepared in example one, example two, example three, example four, comparative example one, comparative example two, comparative example three, and comparative example four in the experimental group;
FIG. 3 is a graph showing the current efficiency of PCB plates treated with electroplating additives prepared in example one, example two, example three, example four, comparative example one, comparative example two, comparative example three and comparative example four in experimental groups;
FIG. 4 is a schematic structural view of the primary brightener.
Detailed Description
For further explanation of the various embodiments, the drawings which form a part of the disclosure and which are incorporated in and constitute a part of this specification, illustrate embodiments and, together with the description, serve to explain the principles of operation of the embodiments, and to enable others of ordinary skill in the art to understand the various embodiments and advantages of the invention, and, by reference to these figures, reference is made to the accompanying drawings, which are not to scale and wherein like reference numerals generally refer to like elements.
According to an embodiment of the present invention, a high stability type plating additive and a method for preparing the same are provided.
Example one
A high-stability electroplating additive comprises the following components in percentage by mass:
100g of copper sulfate pentahydrate;
25g of sulfuric acid;
40g of chloride ions;
20g of a buffering agent;
6g of primary brightening agent;
11g of an emulsifier;
20g of secondary brightening agent;
20g of a softening agent;
1g of inhibitor;
5g of a jar opening agent;
1g of fluorine-containing glycerol ether;
60g of carrier brightener;
1g of microporous nickel additive.
The buffer is boric acid.
The primary brightener is shown in FIG. 4.
The emulsifier comprises sodium allylsulfonate, polyoxyethylene ether and propargyl sodium sulfonate, and the mass fraction ratio is 6:4:1.
the secondary brightening agent comprises 1,4-butynediol, diethoxybutynediol, ethoxypropynol, diethyl propynylamine, and propane pyridine sulfate, and the secondary brightening agent is prepared by a method comprising the steps of:
adding 1,4-butynediol, diethoxybutynediol, ethoxypropynyl alcohol, diethylpropynyl amine, and propidium sulfate sequentially into a reactor;
the mixed liquid is stirred by adjusting the number of jet orifices below the blades of the reactor and the stirring speed;
the secondary brightener is obtained by adding a proper amount of acid into the reactor and reducing the pH value, and controlling the pH value of the mixed solution to be about 7.
The softening agent is an imidazole type softening agent.
The cylinder opening agent comprises the following components in percentage by mass: 1, an aldehyde compound and a manganese-containing compound;
wherein the aldehyde compound is
-a diketone compound;
the manganese-containing compound is high manganese anhydride.
The fluorine-containing glycerol ether is perfluorononene polyglycerol ether.
The carrier brightening agent is a nonionic polyether compound.
Selecting the raw materials with the mass fraction, and preparing the electroplating additive according to a preparation method of the high-stability electroplating additive, as shown in figure 1, wherein the preparation method comprises the following steps:
s1, weighing a proper amount of blue copperas solution, adding the blue copperas solution into deionized water, stirring and dissolving, adding required amount of sulfuric acid and chloride ions, and stirring uniformly to obtain a base solution;
s2, putting the base solution into a reactor, and setting plating conditions of the reactor;
s3, sequentially adding a buffering agent, a primary brightening agent, an emulsifying agent and a secondary brightening agent into the base liquid while stirring, and controlling the stirring speed to be 2000rpm/min;
and S4, regulating and controlling the reaction temperature of the reactor, controlling the temperature at room temperature, sequentially adding a softening agent, an inhibitor, a cylinder opening agent, fluorine-containing glyceryl ether and a carrier brightener, and uniformly stirring to obtain the high-stability electroplating additive.
Example two
A high-stability electroplating additive comprises the following components in percentage by mass:
150g of copper sulfate pentahydrate;
32.5g of sulfuric acid;
60g of chloride ions;
50g of a buffering agent;
9g of primary brightening agent;
27.5g of emulsifier;
40g of secondary brightener;
22.5g of a softening agent;
5.5g of inhibitor;
10g of a jar opening agent;
5.5g of fluorine-containing glycerol ether;
80g of carrier brightener;
5.5g of microporous nickel additive.
The buffer is boric acid.
The primary brightener is shown in FIG. 4.
The emulsifier comprises sodium allylsulfonate, polyoxyethylene ether and propargyl sodium sulfonate, and the mass fraction ratio is 6:4:1.
the secondary brightening agent comprises 1,4-butynediol, diethoxybutynediol, ethoxypropynol, diethyl propynylamine, and propane pyridine sulfate, and the secondary brightening agent is prepared by a method comprising the steps of:
adding 1,4-butynediol, diethoxybutynediol, ethoxypropynyl alcohol, diethylpropynyl amine, and propidium sulfate sequentially into a reactor;
the mixed liquid is stirred by adjusting the number of jet ports below the blades of the reactor and the stirring speed;
the secondary brightener is obtained by adding a proper amount of acid into the reactor and reducing the pH value, and controlling the pH value of the mixed solution to be about 7.
The softening agent is an imidazole type softening agent.
The cylinder opening agent comprises the following components in percentage by mass: 1, an aldehyde compound and a manganese-containing compound;
wherein the aldehyde compound is
-a diketone compound;
the manganese-containing compound is manganese acid anhydride.
The fluorine-containing glycerol ether is perfluorononene polyglycerol ether.
The carrier brightening agent is a nonionic polyether compound.
Selecting the raw materials with the mass fraction, and preparing the electroplating additive according to a preparation method of the high-stability electroplating additive, wherein the preparation method comprises the following steps:
s1, weighing a proper amount of blue copperas solution, adding the blue copperas solution into deionized water, stirring and dissolving, adding required amount of sulfuric acid and chloride ions, and stirring uniformly to obtain a base solution;
s2, putting the base solution into a reactor, and setting plating conditions of the reactor;
s3, sequentially adding a buffering agent, a primary brightening agent, an emulsifying agent and a secondary brightening agent into the base liquid while stirring, and controlling the stirring speed to be 2000rpm/min;
and S4, regulating and controlling the reaction temperature of the reactor, controlling the temperature at room temperature, sequentially adding a softening agent, an inhibitor, a cylinder opening agent, fluorine-containing glyceryl ether and a carrier brightener, and uniformly stirring to obtain the high-stability electroplating additive.
EXAMPLE III
A high-stability electroplating additive comprises the following components in percentage by mass:
200g of blue vitriol;
40g of sulfuric acid;
80g of chloride ions;
80g of buffering agent;
12g of primary brightening agent;
44g of emulsifier;
60g of secondary brightener;
25g of a softening agent;
10g of inhibitor;
15g of a jar opening agent;
10g of fluorine-containing glycerol ether;
100g of carrier brightener.
Microporous nickel additive 10g
The buffer is boric acid.
The primary brightener is shown in FIG. 4.
The emulsifier comprises sodium allylsulfonate, polyoxyethylene ether and propargyl sodium sulfonate, and the mass fraction ratio is 6:4:1.
the secondary brightening agent includes 1,4-butynediol, diethoxybutynediol, ethoxypropynyl alcohol, diethylpropynyl amine, and propane sulfate pyridine, and the method for preparing the secondary brightening agent includes the steps of:
adding 1,4-butynediol, diethoxybutynediol, ethoxypropynyl alcohol, diethylpropynyl amine, and propidium sulfate sequentially into a reactor;
the mixed liquid is stirred by adjusting the number of jet ports below the blades of the reactor and the stirring speed;
the secondary brightener is obtained by adding a proper amount of acid into the reactor and reducing the pH value, and controlling the pH value of the mixed solution to be about 7.
The softening agent is ester-based quaternary ammonium salt.
The cylinder opening agent comprises the following components in percentage by mass: 1, an aldehyde compound and a manganese-containing compound;
wherein the aldehyde compound is acetaldehyde propylene glycol acetal;
the manganese-containing compound is manganese naphthenate.
The fluorine-containing glycerol ether is octafluorobiphenyl diglycidyl ether.
The carrier brightening agent is fatty alcohol-polyoxyethylene ether.
Selecting the raw materials with the mass fraction, and preparing the electroplating additive according to a preparation method of the high-stability electroplating additive, wherein the preparation method comprises the following steps:
s1, weighing a proper amount of blue copperas solution, adding the blue copperas solution into deionized water, stirring and dissolving, adding required amount of sulfuric acid and chloride ions, and stirring uniformly to obtain a base solution;
s2, putting the base solution into a reactor, and setting plating conditions of the reactor;
s3, sequentially adding a buffering agent, a primary brightening agent, an emulsifying agent and a secondary brightening agent into the base liquid while stirring, and controlling the stirring speed to be 2000rpm/min;
and S4, regulating and controlling the reaction temperature of the reactor, controlling the temperature at room temperature, sequentially adding a softening agent, an inhibitor, a cylinder opening agent, fluorine-containing glyceryl ether and a carrier brightener, and uniformly stirring to obtain the high-stability electroplating additive.
Comparative example 1
A high-stability electroplating additive comprises the following components in percentage by mass:
100g of copper sulfate pentahydrate;
25g of sulfuric acid;
40g of chloride ions;
20g of buffering agent;
6g of primary brightening agent;
11g of an emulsifier;
20g of secondary brightening agent;
5g of a jar opening agent;
1g of fluorine-containing glycerol ether;
60g of carrier brightener;
1g of microporous nickel additive.
The buffer is boric acid.
The primary brightener is shown in fig. 4.
The emulsifier comprises sodium allylsulfonate, polyoxyethylene ether and sodium propargyl sulfonate, and the mass fraction ratio is 6:4:1.
the secondary brightening agent includes 1,4-butynediol, diethoxybutynediol, ethoxypropynyl alcohol, diethylpropynyl amine, and propane sulfate pyridine, and the method for preparing the secondary brightening agent includes the steps of:
adding 1,4-butynediol, diethoxybutynediol, ethoxypropynyl alcohol, diethylpropynyl amine, and propidium sulfate sequentially into a reactor;
the mixed liquid is stirred by adjusting the number of jet ports below the blades of the reactor and the stirring speed;
the secondary brightener is obtained by adding a proper amount of acid into the reactor and reducing the pH value, and controlling the pH value of the mixed solution to be about 7.
The softening agent is dialkyl quaternary ammonium salt.
The cylinder opening agent comprises the following components in percentage by mass: 1, an aldehyde compound and a manganese-containing compound;
wherein the aldehyde compound is dimethoxymethane;
the manganese-containing compound is manganese carbonate.
The fluorine-containing glycidyl ether is hexadecafluorononyl glycidyl ether.
The carrier brightening agent is a nonionic polyether compound.
Selecting the raw materials with the mass fraction, and preparing the electroplating additive according to a preparation method of the high-stability electroplating additive, wherein the preparation method comprises the following steps:
s1, weighing a proper amount of blue copperas solution, adding the blue copperas solution into deionized water, stirring and dissolving, adding required amount of sulfuric acid and chloride ions, and stirring uniformly to obtain a base solution;
s2, putting the base solution into a reactor, and setting plating conditions of the reactor;
s3', adding a buffering agent, a primary brightening agent and an emulsifying agent into the base liquid in sequence while stirring, and controlling the stirring speed to be 2000rpm/min;
and S4', regulating and controlling the reaction temperature of the reactor, controlling the temperature at room temperature, sequentially adding an inhibitor, a cylinder opening agent, fluorine-containing glycerol ether and a carrier brightener, and uniformly stirring to obtain the high-stability electroplating additive.
Comparative example No. two
A high-stability electroplating additive comprises the following components in percentage by mass:
100g of copper sulfate pentahydrate;
25g of sulfuric acid;
40g of chloride ions;
20g of a buffering agent;
20g of secondary brightening agent;
11g of an emulsifier;
1g of inhibitor;
5g of a jar opening agent;
1g of fluorine-containing glycerol ether;
1g of microporous nickel additive.
The buffer is boric acid.
The emulsifier comprises sodium allylsulfonate, polyoxyethylene ether and propargyl sodium sulfonate, and the mass fraction ratio is 6:4:1.
the secondary brightening agent includes 1,4-butynediol, diethoxybutynediol, ethoxypropynyl alcohol, diethylpropynyl amine, and propane sulfate pyridine, and the method for preparing the secondary brightening agent includes the steps of:
adding 1,4-butynediol, diethoxybutynediol, ethoxypropynyl alcohol, diethylpropynyl amine, and propidium sulfate sequentially into a reactor;
the mixed liquid is stirred by adjusting the number of jet ports below the blades of the reactor and the stirring speed;
the secondary brightener is obtained by adding a proper amount of acid into the reactor and reducing the pH value, and controlling the pH value of the mixed solution to be about 7.
The softening agent is an imidazole type softening agent.
The cylinder opening agent comprises the following components in percentage by mass: 1, an aldehyde compound and a manganese-containing compound;
wherein the aldehyde compound is 2-methylpropionaldehyde;
the manganese-containing compound is basic manganese oxide.
The fluorine-containing glycerol ether is perfluorononene polyglycerol ether.
The carrier brightening agent is a nonionic polyether compound.
Selecting the raw materials with the mass fraction, and preparing the electroplating additive according to a preparation method of the high-stability electroplating additive, wherein the preparation method comprises the following steps:
s1, weighing a proper amount of blue copperas solution, adding the blue copperas solution into deionized water, stirring and dissolving, adding required amount of sulfuric acid and chloride ions, and stirring uniformly to obtain a base solution;
s2, putting the base solution into a reactor, and setting plating conditions of the reactor;
s3', adding a buffering agent, a primary brightening agent and an emulsifying agent into the base liquid in sequence while stirring, and controlling the stirring speed to be 2000rpm/min;
and S4', regulating and controlling the reaction temperature of the reactor, controlling the temperature at room temperature, sequentially adding an inhibitor, a cylinder opening agent and fluorine-containing glycerol ether, and uniformly stirring to obtain the high-stability electroplating additive.
Comparative example No. three
A high-stability electroplating additive comprises the following components in percentage by mass:
100g of copper sulfate pentahydrate;
25g of sulfuric acid;
40g of chloride ions;
20g of a buffering agent;
20g of secondary brightening agent;
1g of inhibitor;
5g of a jar opening agent;
1g of fluorine-containing glycerol ether;
1g of microporous nickel additive.
The buffer is boric acid.
The emulsifier comprises sodium allylsulfonate, polyoxyethylene ether and propargyl sodium sulfonate, and the mass fraction ratio is 6:4:1.
the secondary brightening agent includes 1,4-butynediol, diethoxybutynediol, ethoxypropynyl alcohol, diethylpropynyl amine, and propane sulfate pyridine, and the method for preparing the secondary brightening agent includes the steps of:
1,4-butynediol, diethoxybutynediol, ethoxypropynyl alcohol, diethylpropynyl amine, and propidium sulfate are sequentially added into a reactor;
the mixed liquid is stirred by adjusting the number of jet orifices below the blades of the reactor and the stirring speed;
the secondary brightener is obtained by adding a proper amount of acid into the reactor and reducing the pH value, and controlling the pH value of the mixed solution to be about 7.
The cylinder opening agent comprises the following components in percentage by mass: 1 aldehyde compound and manganese-containing compound;
wherein the aldehyde compound is
-a diketone compound;
the manganese-containing compound is high manganese anhydride.
The fluorine-containing glycerol ether is perfluorononene polyglycerol ether.
Selecting the raw materials with the mass fraction, and preparing the electroplating additive according to a preparation method of the high-stability electroplating additive, wherein the preparation method comprises the following steps:
s1, weighing a proper amount of blue copperas solution, adding the blue copperas solution into deionized water, stirring and dissolving, adding required amount of sulfuric acid and chloride ions, and stirring uniformly to obtain a base solution;
s2, putting the base solution into a reactor, and setting plating conditions of the reactor;
s3', adding a buffering agent and a primary brightening agent into the base liquid in sequence while stirring, and controlling the stirring speed to be 2000rpm/min;
and S4', regulating and controlling the reaction temperature of the reactor, controlling the temperature at room temperature, sequentially adding an inhibitor, a cylinder opening agent and fluorine-containing glyceryl ether, and uniformly stirring to obtain the high-stability electroplating additive.
Comparative example No. four
The secondary brightening agent includes 1,4-butynediol, diethoxybutynediol, ethoxypropynyl alcohol, diethylpropynyl amine, and propane sulfate pyridine, and the method for preparing the secondary brightening agent includes the steps of:
adding 1,4-butynediol, diethoxybutynediol, ethoxypropynyl alcohol, diethylpropynyl amine, and propidium sulfate sequentially into a reactor;
the mixed liquid is stirred by adjusting the number of jet ports below the blades of the reactor and the stirring speed;
the secondary brightener is obtained by adding a proper amount of acid into the reactor and reducing the pH value, and controlling the pH value of the mixed solution to be about 7.
The cylinder opening agent comprises the following components in percentage by mass: 1 aldehyde compound and manganese-containing compound;
wherein the aldehyde compound is
-a diketone compound;
the manganese-containing compound is high manganese anhydride.
The carrier brightening agent is a nonionic polyether compound.
Selecting the raw materials with the mass fraction, and preparing the electroplating additive according to a preparation method of the high-stability electroplating additive, wherein the preparation method comprises the following steps:
s1, weighing a proper amount of blue copperas solution, adding the blue copperas solution into deionized water, stirring and dissolving, adding required amount of sulfuric acid and chloride ions, and stirring uniformly to obtain a base solution;
s2, putting the base solution into a reactor, and setting plating conditions of the reactor;
s3', adding a buffering agent and a secondary brightening agent into the base solution in sequence while stirring, and controlling the stirring speed to be 2000rpm/min;
and S4' ' ', regulating and controlling the reaction temperature of the reactor, controlling the temperature at room temperature, sequentially adding a cylinder opening agent, and uniformly stirring to obtain the high-stability electroplating additive.
Experimental group
Respectively selecting the electroplating additives prepared in the first embodiment, the second embodiment, the third embodiment, the fourth embodiment, the first comparative embodiment, the second comparative embodiment, the third comparative embodiment and the fourth comparative embodiment, placing the electroplating additives in a container, adding PCB boards with the same specification for electroplating reaction, observing experimental phenomena and recording experimental data, wherein the experimental results are shown in Table 1, FIG. 2 and FIG. 3;
table 1: comparison table of electroplating performance of each example and comparative example
| Hardness (HV) | Current efficiency (%) | Brightness (grade) | PCB qualification rate (%) | |
| Example one | 260 | 99.2 | 4 | 98.4 |
| Example two | 254 | 99.4 | 4 | 98.6 |
| EXAMPLE III | 240 | 99.2 | 4 | 98.4 |
| Comparative example 1 | 210 | 98 | 4 | 97.1 |
| Comparative example No. two | 220 | 97.5 | 3 | 95.2 |
| Comparative example No. three | 200 | 97.4 | 2 | 94.4 |
| Comparative example No. four | 190 | 98.1 | 2 | 86 |
As can be seen from Table 1, the electroplating additive prepared by the method has the functional advantages of high stability and high brightness, and the processing quantity and the qualification rate of PCBs are obviously improved.
In conclusion, by means of the technical scheme, the performance of the plating solution and the plating layer is improved to a great extent by adding the emulsifier, the secondary brightener, the primary brightener, the carrier brightener and the like, and the additive can not generate impurities in the plating layer, so that the surface brightness of the plating layer can be obviously improved, and the uniformity of the plating layer is ensured; the nickel plating process containing the multilayer nickel electroplating additive provided by the invention adopts a smaller current density, reduces the energy consumption, has short electroplating time, good bright effect after nickel plating and high stability.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The high-stability electroplating additive is characterized by comprising the following components in percentage by mass:
100-200 parts of copper sulfate pentahydrate;
25-40 parts of sulfuric acid;
40-80 parts of chloride ions;
20-80 parts of a buffering agent;
6-12 parts of a primary brightening agent;
11-44 parts of an emulsifier;
20-60 parts of a secondary brightening agent;
20-25 parts of a softening agent;
1-10 parts of an inhibitor;
5-15 parts of a jar opening agent;
1-10 parts of fluorine-containing glycerol ether;
60-100 parts of a carrier brightener;
1-10 parts of a microporous nickel additive.
2. A highly stable electroplating additive as claimed in claim 1, wherein said buffer comprises boric acid, phosphoric acid, citric acid, carbonic acid, acetic acid and barbituric acid.
3. The high stability type plating additive as claimed in claim 1, wherein the primary brightenerIs containing = C-SO 2 -an organic compound of structure.
4. The high-stability electroplating additive according to claim 1, wherein the emulsifier comprises sodium allyl sulfonate, polyoxyethylene ether and sodium propargyl sulfonate, and the mass ratio of the sodium allyl sulfonate to the polyoxyethylene ether is 6:4:1.
5. the additive as recited in claim 1 wherein said secondary brighteners comprise 1,4-butynediol, diethoxybutynediol, ethoxypropynol, diethylpropynylamine, and pyridinium sulfate.
6. A high stability additive package as set forth in claim 1, wherein said softening agent comprises esterquat, dialkylquat, alkylacylquat, pyridinium quat and imidazole type softening agents.
7. The high stability electroplating additive as recited in claim 1 wherein the cylinder opener comprises, by mass, 1:1, an aldehyde compound and a manganese-containing compound;
wherein the aldehyde compounds comprise acetaldehyde propylene glycol acetal, phenylpropargyl aldehyde acetal, and,
-diketone compounds, dimethoxymethane, p-methoxybenzaldehyde, 2-furylaldehyde, 2-methylpropionaldehyde and p-dimethylaminobenzaldehyde;
the manganese-containing compound comprises manganese naphthenate, manganous anhydride, manganese anhydride, basic manganese oxide, manganese carbonate and high manganese anhydride.
8. The additive for electroplating of claim 1, wherein said fluorinated glycerol ether comprises perfluorononene polyglycerol ether, octafluorobiphenyl diglycidyl ether, and hexadecafluorononyl glycidyl ether.
9. A high stability type plating additive according to claim 1, wherein said carrier brightener is fatty alcohol polyoxyethylene ether.
10. A method for preparing a high stability type electroplating additive according to any one of claims 1-9, wherein the method comprises the following steps:
s1, weighing a proper amount of blue copperas solution, adding the blue copperas solution into deionized water, stirring and dissolving, adding required amount of sulfuric acid and chloride ions, and stirring uniformly to obtain a base solution;
s2, putting the base solution into a reactor, and setting plating conditions of the reactor;
s3, sequentially adding a buffering agent, a primary brightening agent, an emulsifying agent and a secondary brightening agent into the base liquid while stirring, and controlling the stirring speed to be 2000rpm/min;
and S4, regulating and controlling the reaction temperature of the reactor, controlling the temperature at room temperature, sequentially adding a softening agent, an inhibitor, a cylinder opening agent, fluorine-containing glyceryl ether, a carrier brightening agent and a microporous nickel additive, and uniformly stirring to obtain the high-stability electroplating additive.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB949016A (en) * | 1962-07-09 | 1964-02-05 | Langbein Pfanhauser Werke Ag | Electrolytic deposition of bright metal coatings |
| GB1213267A (en) * | 1968-05-31 | 1970-11-25 | Nickel Le | Improvements in or relating to high-rate electrolytic nickel-plating methods, and installations |
| JPS50116332A (en) * | 1974-02-19 | 1975-09-11 | ||
| CN101273157A (en) * | 2005-06-20 | 2008-09-24 | 百富可公司 | Zinc-nickel alloy electroplating system |
| US20150090600A1 (en) * | 2012-04-19 | 2015-04-02 | Dipsol Chemicals Co., Ltd. | Copper-nickel alloy electroplating bath and plating method |
| CN109609979A (en) * | 2019-02-19 | 2019-04-12 | 广州睿邦新材料科技有限公司 | A kind of multi layer nickel plating additive improving stability |
-
2022
- 2022-11-21 CN CN202211455891.0A patent/CN115787053A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB949016A (en) * | 1962-07-09 | 1964-02-05 | Langbein Pfanhauser Werke Ag | Electrolytic deposition of bright metal coatings |
| GB1213267A (en) * | 1968-05-31 | 1970-11-25 | Nickel Le | Improvements in or relating to high-rate electrolytic nickel-plating methods, and installations |
| JPS50116332A (en) * | 1974-02-19 | 1975-09-11 | ||
| CN101273157A (en) * | 2005-06-20 | 2008-09-24 | 百富可公司 | Zinc-nickel alloy electroplating system |
| US20150090600A1 (en) * | 2012-04-19 | 2015-04-02 | Dipsol Chemicals Co., Ltd. | Copper-nickel alloy electroplating bath and plating method |
| CN109609979A (en) * | 2019-02-19 | 2019-04-12 | 广州睿邦新材料科技有限公司 | A kind of multi layer nickel plating additive improving stability |
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