CN115478267A - Intelligent preparation process of electroless copper plating solution applied to PCB - Google Patents
Intelligent preparation process of electroless copper plating solution applied to PCB Download PDFInfo
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- CN115478267A CN115478267A CN202211154448.XA CN202211154448A CN115478267A CN 115478267 A CN115478267 A CN 115478267A CN 202211154448 A CN202211154448 A CN 202211154448A CN 115478267 A CN115478267 A CN 115478267A
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/18—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material
- H05K3/181—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material by electroless plating
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Abstract
The invention discloses an intelligent preparation process of a chemical copper plating solution applied to a PCB, which comprises the following steps: s1, dissolving 30-60 parts of blue vitriod in water, cleaning and filtering to obtain a blue vitriod solution; s2, sequentially adding 35-50 parts of additive, 40-70 parts of reducing agent, 20-40 parts of complexing agent, 6-15 parts of stabilizer, 8-15 parts of accelerator and 2-5 parts of surfactant into the copper sulfate solution by using an automatic adding instrument, and uniformly stirring to obtain a mixed solution; s3, adding a proper amount of pH regulator into the mixed solution by using an automatic adding instrument; and S4, measuring the parameters of the mixed solution by using monitoring equipment. The invention intelligently controls the chemical copper plating solution preparation process by constructing the fuzzy controller, can carry out real-time monitoring and capturing aiming at the change of each parameter in the copper plating solution, and then carries out fuzzy control of automatic addition of each component by utilizing the fuzzy control rule to feed back, thereby forming an automatic intelligent preparation flow.
Description
Technical Field
The invention relates to the technical field of chemical copper plating solutions, in particular to an intelligent preparation process of a chemical copper plating solution applied to a PCB.
Background
Electroless copper plating has wide application in the metallization of holes in Printed Circuit Boards (PCB), the metallization of plastic and ceramic surfaces, the preparation of electromagnetic shielding materials, and the like. Electroless plating is a metal deposition process in which metal ions are reduced by a suitable reducing agent in solution under the autocatalytic action of the metal surface, and electroless plating can only be performed on catalytically active surfaces. The method for forming metal or metal layer on the plated part with catalytic activity by using chemical reducing agent has the advantages of no need of power supply, simple process equipment, uniform plating thickness and good bonding force, and can be carried out on the surfaces of non-metals (non-conductors) such as plastics, glass, ceramics and semiconductor materials. Based on the characteristic that chemical plating is superior to electroplating, the method is widely applied to the field of circuit board manufacturing.
Electroless copper plating solutions are widely varied. The copper plating layer is divided into a thin copper plating solution and a thick copper plating solution according to the thickness of the copper plating layer (namely, the deposition rate is required to reach 6-9 mu m/h, and the thickness of the plating layer reaches 2-3 mu m within 30 min); the solutions can be classified into plastic metallization, hole metallization of printed circuit boards, and the like according to the application of the solutions. The chemical copper plating solution mainly comprises copper salt, a reducing agent, a complexing agent, a stabilizing agent, a pH value regulator and other additives. Electroless plating is the controlled autocatalytic deposition of a continuous film of metal without the assistance of an external electron supply. Non-metallic surfaces may be pre-treated to make them receptive or catalytic for deposition. All or selected portions of the surface may be suitably pretreated. The complexing agent serves to chelate the copper to be deposited and prevent the copper from precipitating out of solution. Copper chelated makes copper available to reducing agents that convert copper ions to metallic form.
At present, the development trend of circuit board production is a chemical copper plating process for directly metalizing a circuit board, and the process comprises the following steps: the substrate is selectively activated to form a patterned activated area, and then copper is deposited on the activated area in an electroless copper plating solution to form a conductive trace. When chemical copper plating solution is prepared at present, solid raw materials such as copper sulfate pentahydrate, potassium sodium tartrate and ethylene diamine tetraacetic acid often contain certain impurities, and when the solid raw materials are dissolved in the solution, the impurities can be mixed with the solution, so that the quality of the copper plating solution is reduced, and further the copper plating of a PCB (printed circuit board) can be influenced; meanwhile, the traditional preparation process lacks intelligent control, the high consistency of the finished products prepared in batches and a set value cannot be guaranteed, and the preparation components are not improved aiming at the defects in the prior art, so that the functional purposes of intelligent and efficient preparation, low labor capacity, no pollution and excellent finished product effect are achieved.
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 an intelligent preparation process of a chemical copper plating solution applied to a PCB (printed Circuit Board), so as to overcome the technical problems in the prior related art.
Therefore, the invention adopts the following specific technical scheme:
an intelligent preparation process of electroless copper plating solution applied to a PCB comprises the following steps:
s1, dissolving 30-60 parts of blue vitriod in water, cleaning and filtering to obtain a blue vitriod solution;
s2, sequentially adding 35-50 parts of additive, 40-70 parts of reducing agent, 20-40 parts of complexing agent, 6-15 parts of stabilizer, 8-15 parts of accelerator and 2-5 parts of surfactant into the copper sulfate solution by using an automatic adding instrument, and uniformly stirring to obtain a mixed solution;
s3, adding a proper amount of pH regulator into the mixed solution by using an automatic adding instrument;
s4, measuring parameters of the mixed solution by using monitoring equipment;
s5, controlling the parameters of the mixed solution by using a fuzzy controller, and adjusting the operation of each automatic adding instrument until the parameters meet a set value range;
and S6, cleaning the prepared mixed solution by using hydrogen peroxide, and filtering to remove impurities to obtain the final chemical copper plating solution.
Further, the method for preparing the copper sulfate solution by dissolving 30-60 parts of blue copperas in water and cleaning and filtering comprises the following steps:
s11, weighing 30-60 parts of blue vitriod, placing in deionized water at 40-60 ℃, and stirring until the blue vitriod is completely dissolved;
s12, adding activated carbon into the completely dissolved solution, standing for 10-20h, and filtering;
and S13, adding sulfuric acid into the filtered solution and uniformly stirring to obtain a copper sulfate solution.
Further, the additive comprises at least two of thiourea, 2,2-bipyridine, L-arginine and potassium ferrocyanide;
the complexing agent comprises ethylene diamine tetraacetic acid and triethanolamine, and the mass portion ratio is 1:1.
further, the reducing agent comprises glyoxylic acid and glyoxylic acid, and the mass part ratio of the glyoxylic acid to the glyoxylic acid is 2:5.
further, the stabilizer comprises sodium sulfite and polyoxyethylene sorbitan monostearate (Tween-60) and the mass part ratio of the sodium sulfite to the polyoxyethylene sorbitan monostearate is 1:4.
further, the surfactant is tween-80;
the accelerator comprises at least one of aminopyridine, ammonium chloride, nickel sulfate, ferrous sulfate, cytosine, 2-mercaptobenzothiazole, adenine and benzotriazole.
Further, the pH regulator comprises sodium hydroxide and sodium carbonate, and the pH value is between 11.8 and 12.7.
Furthermore, the monitoring equipment comprises a temperature sensor, a pH meter probe and a photoelectric colorimeter; the parameters include copper ion concentration, pH and temperature.
Further, the fuzzy controller comprises a database, a knowledge base, a fuzzy control rule set and a fuzzy logic reasoning unit;
the database is used for storing parameters and production data in the preparation process;
the knowledge base is used for storing professional technical knowledge;
the fuzzy control rule set is used for constructing and storing fuzzy control rules to meet the requirements of the preparation process aiming at the characteristics of the change of the electroless copper plating solution;
and the fuzzy logic reasoning unit is used for matching a corresponding fuzzy control rule according to the current parameter and the control state and outputting fuzzy control.
Further, the control states include:
in the formula (I), the compound is shown in the specification,
representing the characteristic state of the fuzzy controller,
the deviation of the system is shown as such,Ra given value of the parameter is represented,Yindicating the current value of E is added.
The invention has the beneficial effects that:
1. the preparation process of the chemical copper plating solution is intelligently controlled by constructing the fuzzy controller, real-time monitoring and capturing can be carried out on the change of each parameter in the copper plating solution, and fuzzy control of automatic addition of each component is carried out by feedback according to a fuzzy control rule, so that an automatic intelligent preparation process is formed, the preset basic parameters of the chemical copper plating solution are met, and the aims of high-speed response, flexible control and accurate preparation are fulfilled.
2. The prepared copper sulfate solution is washed by activated carbon in advance, so that the purity of the copper sulfate solution can be effectively improved, and the contents of impurities and redundant ions in the copper sulfate solution are reduced and removed, so that the copper plating film performance of the copper plating solution is improved; and after the preparation is finished, impurities in the copper plating solution can be effectively removed by cleaning with hydrogen peroxide, so that the solution is maintained and stabilized, and the service life of the copper plating solution is effectively prolonged.
3. The reducing agent prepared by mixing glyoxylic acid and glyoxylic acid is matched with the additive, and the complexing agent quantitatively prepared from ethylenediamine tetraacetic acid and triethanolamine is matched, so that the deposition rate of the copper plating solution can be greatly improved, the efficiency of the copper plating solution is ensured, and meanwhile, the flatness and the brightness of the surface of the PCB can be greatly improved through the surfactant, so that the PCB with uniform, bright and smooth floating layer is formed.
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 an intelligent preparation process of electroless copper plating solution applied to a PCB according to an embodiment of the invention;
FIG. 2 is a schematic diagram showing the comparison of plating rates of electroless plating solutions according to examples one, two, three, four and five in the experimental examples of the present invention and comparative examples one, two and three;
FIG. 3 is a graph showing the decomposition time of electroless plating solutions according to examples one, two, three, four, five and comparative examples one, two, three in the experimental example of the present invention;
FIG. 4 is a schematic diagram showing the comparison of the plating thickness of the electroless plating solutions of the first, second, third, fourth, and fifth examples and the first, second, and third comparative examples on a PCB according to the experimental example of the present invention.
Detailed Description
According to the embodiment of the present invention, as shown in fig. 1, an intelligent preparation process of electroless copper plating solution for PCB is provided, and the preparation process and the electroless copper plating solution of the present invention will be described in detail with reference to various embodiments.
Example one
An intelligent preparation process of electroless copper plating solution applied to a PCB comprises the following steps:
s1, dissolving 30g of blue copperas in water, cleaning and filtering to obtain a blue copperas solution, comprising the following steps:
s11, weighing 30g of blue vitriod, placing in deionized water (3L) at 50 ℃, and stirring until the blue vitriod is completely dissolved;
s12, adding activated carbon into the completely dissolved solution, standing for 20 hours, and filtering;
s13, adding 15g of sulfuric acid into the filtered solution, and uniformly stirring to obtain a copper sulfate solution.
S2, sequentially adding 35g of additive, 40g of reducing agent, 20g of complexing agent, 6g of stabilizing agent, 8g of accelerating agent and 2g of surfactant into the copper sulfate solution by using an automatic adding instrument (a medicine adding pump is selected as the automatic adding instrument to realize automatic quantitative conveying of component raw materials), and uniformly stirring to obtain a mixed solution;
s3, adding a proper amount of pH regulator into the mixed solution by using an automatic adding instrument;
s4, measuring parameters of the mixed solution by using monitoring equipment;
s5, controlling parameters of the mixed solution by using a fuzzy controller, and adjusting the operation of each automatic adding instrument until the parameters meet a set value range;
and S6, cleaning the prepared mixed solution by using hydrogen peroxide, and filtering to remove impurities to obtain the final chemical copper plating solution.
Wherein the additive comprises thiourea and 2,2-bipyridine;
the complexing agent comprises ethylene diamine tetraacetic acid and triethanolamine, and the mass portion ratio is 1:1.
the reducing agent comprises glyoxylic acid and glyoxylic acid, and the mass part ratio of the glyoxylic acid to the glyoxylic acid is 2:5.
the stabilizer comprises sodium sulfite and polyoxyethylene sorbitan monostearate (Tween-60) and the mass portion ratio is 1:4.
the surfactant is tween-80;
the accelerator includes aminopyridine and ammonium chloride.
The pH regulator comprises sodium hydroxide and sodium carbonate, the pH value is between 12.5, and the temperature of the preparation process is 50 ℃.
In addition, a fuzzy controller is utilized to monitor the preparation process of the copper plating solution, and the control and addition are carried out according to the preset value content of each component, so as to prepare and obtain the complete chemical plating solution.
Example two
An intelligent preparation process of electroless copper plating solution applied to a PCB comprises the following steps:
s1, dissolving 40g of blue copperas in water, cleaning and filtering to obtain a blue copperas solution, comprising the following steps:
s11, weighing 40g of copper sulfate pentahydrate, placing the copper sulfate pentahydrate into deionized water (3L) at 50 ℃, and stirring until the copper sulfate pentahydrate is completely dissolved;
s12, adding activated carbon into the completely dissolved solution, standing for 20 hours, and filtering;
s13, adding 15g of sulfuric acid into the filtered solution, and uniformly stirring to obtain a copper sulfate solution.
S2, adding 40g of additive, 50g of reducing agent, 28g of complexing agent, 9g of stabilizing agent, 10g of accelerator and 3g of surfactant into the copper sulfate solution in sequence by using an automatic adding instrument, and uniformly stirring to obtain a mixed solution;
s3, adding a proper amount of pH regulator into the mixed solution by using an automatic adding instrument;
s4, measuring parameters of the mixed solution by using monitoring equipment;
s5, controlling parameters of the mixed solution by using a fuzzy controller, and adjusting the operation of each automatic adding instrument until the parameters meet a set value range;
and S6, cleaning the prepared mixed solution by using hydrogen peroxide, and filtering to remove impurities to obtain the final chemical copper plating solution.
Wherein the additive comprises thiourea and 2,2-bipyridine;
the complexing agent comprises ethylene diamine tetraacetic acid and triethanolamine, and the mass portion ratio is 1:1.
the reducing agent comprises glyoxylic acid and glyoxylic acid, and the mass part ratio of the glyoxylic acid to the glyoxylic acid is 2:5.
the stabilizer comprises sodium sulfite and polyoxyethylene sorbitan monostearate (Tween-60) in a mass part ratio of 1:4.
the surfactant is tween-80;
the accelerator includes an aminopyridine and ammonium chloride.
The pH regulator comprises sodium hydroxide and sodium carbonate, the pH value is between 12.5, and the temperature of the preparation process is 50 ℃.
In addition, a fuzzy controller is utilized to monitor the preparation process of the copper plating solution, and the control and addition are carried out according to the preset value content of each component, so as to prepare and obtain the complete chemical plating solution.
EXAMPLE III
An intelligent preparation process of electroless copper plating solution applied to a PCB comprises the following steps:
s1, dissolving 50g of blue copperas in water, cleaning and filtering to obtain a blue copperas solution, comprising the following steps:
s11, weighing 50g of copper sulfate pentahydrate, placing the copper sulfate pentahydrate into deionized water (3L) at 50 ℃, and stirring until the copper sulfate pentahydrate is completely dissolved;
s12, adding activated carbon into the completely dissolved solution, standing for 20 hours, and filtering;
s13, adding 15g of sulfuric acid into the filtered solution, and uniformly stirring to obtain a copper sulfate solution.
S2, adding 45g of additive, 60g of reducing agent, 35g of complexing agent, 12g of stabilizing agent, 12g of accelerator and 4g of surfactant into the copper sulfate solution in sequence by using an automatic adding instrument, and uniformly stirring to obtain a mixed solution;
s3, adding a proper amount of pH regulator into the mixed solution by using an automatic adding instrument;
s4, measuring parameters of the mixed solution by using monitoring equipment;
s5, controlling the parameters of the mixed solution by using a fuzzy controller, and adjusting the operation of each automatic adding instrument until the parameters meet a set value range;
and S6, cleaning the prepared mixed solution by using hydrogen peroxide, and filtering to remove impurities to obtain the final chemical copper plating solution.
Wherein the additive comprises thiourea and 2,2-bipyridine;
the complexing agent comprises ethylene diamine tetraacetic acid and triethanolamine, and the mass portion ratio is 1:1.
the reducing agent comprises glyoxylic acid and glyoxylic acid, and the mass part ratio of the glyoxylic acid to the glyoxylic acid is 2:5.
the stabilizer comprises sodium sulfite and polyoxyethylene sorbitan monostearate (Tween-60) and the mass portion ratio is 1:4.
the surfactant is Tween-80;
the accelerator includes aminopyridine and ammonium chloride.
The pH regulator comprises sodium hydroxide and sodium carbonate, the pH value is between 12.5, and the temperature of the preparation process is 50 ℃.
In addition, a fuzzy controller is utilized to monitor the preparation process of the copper plating solution, and the control and addition are carried out according to the preset value content of each component, so as to prepare and obtain the complete chemical plating solution.
Example four
An intelligent preparation process of electroless copper plating solution applied to a PCB comprises the following steps:
s1, dissolving 50g of blue copperas in water, cleaning and filtering to obtain a blue copperas solution, comprising the following steps:
s11, weighing 50g of copper sulfate pentahydrate, placing the copper sulfate pentahydrate into deionized water (3L) at 50 ℃, and stirring until the copper sulfate pentahydrate is completely dissolved;
s12, adding activated carbon into the completely dissolved solution, standing for 20 hours, and filtering;
s13, adding 15g of sulfuric acid into the filtered solution, and uniformly stirring to obtain a copper sulfate solution.
S2, adding 45g of additive, 60g of reducing agent, 35g of complexing agent, 12g of stabilizing agent, 12g of accelerator and 4g of surfactant into the copper sulfate solution in sequence by using an automatic adding instrument, and uniformly stirring to obtain a mixed solution;
s3, adding a proper amount of pH regulator into the mixed solution by using an automatic adding instrument;
s4, measuring parameters of the mixed solution by using monitoring equipment;
s5, controlling parameters of the mixed solution by using a fuzzy controller, and adjusting the operation of each automatic adding instrument until the parameters meet a set value range;
and S6, cleaning the prepared mixed solution by using hydrogen peroxide, and filtering to remove impurities to obtain the final chemical copper plating solution.
Wherein the additive comprises L-arginine and potassium ferrocyanide;
the complexing agent comprises ethylene diamine tetraacetic acid and triethanolamine, and the mass portion ratio is 1:1.
the reducing agent comprises glyoxylic acid and glyoxylic acid, and the mass part ratio of the glyoxylic acid to the glyoxylic acid is 2:5.
the stabilizer comprises sodium sulfite and polyoxyethylene sorbitan monostearate (Tween-60) and the mass portion ratio is 1:4.
the surfactant is tween-80;
the accelerator comprises nickel sulfate, ferrous sulfate and cytosine.
The pH regulator comprises sodium hydroxide and sodium carbonate, the pH value is between 12.5, and the temperature of the preparation process is 50 ℃.
In addition, a fuzzy controller is utilized to monitor the preparation process of the copper plating solution, and the control and addition are carried out according to the preset value content of each component, so as to prepare and obtain the complete chemical plating solution.
EXAMPLE five
An intelligent preparation process of electroless copper plating solution applied to a PCB comprises the following steps:
s1, dissolving 60g of blue copperas in water, cleaning and filtering to obtain a blue copperas solution, comprising the following steps:
s11, weighing 60g of copper sulfate pentahydrate, placing the copper sulfate pentahydrate into deionized water (3L) at 50 ℃, and stirring until the copper sulfate pentahydrate is completely dissolved;
s12, adding activated carbon into the completely dissolved solution, standing for 20 hours, and filtering;
s13, adding 15g of sulfuric acid into the filtered solution, and uniformly stirring to obtain a copper sulfate solution.
S2, sequentially adding 50g of additive, 70g of reducing agent, 40g of complexing agent, 15g of stabilizing agent, 15g of accelerating agent and 5g of surfactant into the copper sulfate solution by using an automatic adding instrument, and uniformly stirring to obtain a mixed solution;
s3, adding a proper amount of pH regulator into the mixed solution by using an automatic adding instrument;
s4, measuring parameters of the mixed solution by using monitoring equipment;
s5, controlling the parameters of the mixed solution by using a fuzzy controller, and adjusting the operation of each automatic adding instrument until the parameters meet a set value range;
and S6, cleaning the prepared mixed solution by using hydrogen peroxide, and filtering to remove impurities to obtain the final chemical copper plating solution.
Wherein the additive comprises thiourea and 2,2-bipyridine;
the complexing agent comprises ethylene diamine tetraacetic acid and triethanolamine, and the mass portion ratio is 1:1.
the reducing agent comprises glyoxylic acid and glyoxylic acid, and the mass part ratio of the glyoxylic acid to the glyoxylic acid is 2:5.
the stabilizer comprises sodium sulfite and polyoxyethylene sorbitan monostearate (Tween-60) and the mass portion ratio is 1:4.
the surfactant is Tween-80;
the accelerator includes aminopyridine and ammonium chloride.
The pH regulator comprises sodium hydroxide and sodium carbonate, the pH value is between 12.5, and the temperature of the preparation process is 50 ℃.
In addition, a fuzzy controller is utilized to monitor the preparation process of the copper plating solution, and the control and addition are carried out according to the preset value content of each component, so as to prepare and obtain the complete chemical plating solution.
Comparative example 1
The traditional preparation process of the electroless copper plating solution applied to the PCB comprises the following steps:
s1, dissolving 50g of blue vitriod in 3L of water, and uniformly mixing to obtain a blue vitriod solution;
s2, adding 45g of additive, 60g of reducing agent, 35g of complexing agent, 12g of stabilizing agent, 12g of accelerator and 4g of surfactant into the copper sulfate solution in sequence by using an automatic adding instrument, and uniformly stirring to obtain a mixed solution;
s3, adding a proper amount of pH regulator into the mixed solution;
and S4, obtaining the prepared electroless copper plating solution.
Wherein the additive comprises thiourea and 2,2-bipyridine;
the complexing agent comprises ethylene diamine tetraacetic acid and triethanolamine, and the mass portion ratio is 1:1.
the reducing agent comprises glyoxylic acid and glyoxylic acid, and the mass part ratio of the glyoxylic acid to the glyoxylic acid is 2:5.
the stabilizer comprises sodium sulfite and polyoxyethylene sorbitan monostearate (Tween-60) and the mass portion ratio is 1:4.
the surfactant is tween-80;
the accelerator includes aminopyridine and ammonium chloride.
The pH regulator comprises sodium hydroxide and sodium carbonate, the pH value is between 12.5, and the temperature of the preparation process is 50 ℃.
Comparative example No. two
The traditional preparation process of the electroless copper plating solution applied to the PCB comprises the following steps:
s1, dissolving 50g of blue vitriod in 3L of water, and uniformly mixing to obtain a blue vitriod solution;
s2, adding 45g of additive, 60g of reducing agent, 35g of complexing agent and 12g of stabilizer into the copper sulfate solution in sequence by using an automatic adding instrument, and uniformly stirring to obtain a mixed solution;
s3, adding a proper amount of pH regulator into the mixed solution;
and S4, obtaining the prepared electroless copper plating solution.
Wherein the additive comprises thiourea and 2,2-bipyridine;
the complexing agent comprises ethylene diamine tetraacetic acid and triethanolamine, and the mass portion ratio is 1:1.
the reducing agent comprises glyoxylic acid and glyoxylic acid, and the mass part ratio of the glyoxylic acid to the glyoxylic acid is 2:5.
the stabilizer comprises sodium sulfite and polyoxyethylene sorbitan monostearate (Tween-60) and the mass portion ratio is 1:4.
the pH regulator comprises sodium hydroxide and sodium carbonate, the pH value is between 12.5, and the temperature of the preparation process is 50 ℃.
Comparative example No. three
The traditional electroless copper plating solution preparation process applied to the PCB comprises the following steps:
s1, dissolving 50g of blue vitriod in 3L of water, and uniformly mixing to obtain a blue vitriod solution;
s2, sequentially adding 45g of additive, 60g of reducing agent, 35g of complexing agent and 12g of stabilizer into the copper sulfate solution by using an automatic adding instrument, and uniformly stirring to obtain a mixed solution;
s3, adding a proper amount of pH regulator into the mixed solution;
and S4, obtaining the prepared electroless copper plating solution.
Wherein the reducing agent is formaldehyde.
The additive, the complexing agent and the stabilizer are all the most common components in the traditional mode.
The pH regulator comprises sodium hydroxide and sodium carbonate, the pH value is between 12.5, and the temperature of the preparation process is 50 ℃.
Examples of the experiments
Selecting 1L of electroless copper plating solution prepared in the first, second, third, fourth and fifth examples and the first, second and third comparative examples, placing the chemical copper plating solution in containers, placing a plurality of pretreated PCB boards in each container respectively for electroless copper plating, synchronously timing and observing, recording copper plating experimental data for comparison, as shown in Table 1 and figures 2-4:
table 1: performance test meter for chemical copper plating solution
| Plating speed (mu m/h) | Plating solution decomposition time (min) | Coating thickness (μm) | Quality of coating | |
| Example one | 14.2 | 105 | 0.31 | Smooth, fine and bright plating layer |
| Example two | 17.5 | 120 | 0.38 | The plating layer is smooth, fine and smooth |
| EXAMPLE III | 22.4 | 154 | 0.44 | The plating layer is level, fine, smooth and bright |
| Example four | 21.8 | 152 | 0.43 | The plating layer is smooth, fine, smooth and bright |
| Practice ofExample five | 20.7 | 147 | 0.40 | The plating layer is smooth, fine and smooth |
| Comparative example 1 | 14.7 | 121 | 0.32 | The plating layer is smooth and even |
| Comparative example No. two | 12.1 | 98 | 0.19 | The coating has rough lines |
| Comparative example No. three | 7.8 | 46 | 0.11 | The coating has rough lines |
As can be seen from table 1 and fig. 2 to 4, the stability of the plating solution can be effectively improved by reasonably configuring, cleaning and filtering the copper plating solution, and the efficiency of the plating solution for plating copper on the PCB is ensured. The traditional copper plating solution can not form a bright and smooth plating layer, obvious short plates exist in the plating layer and the plating speed, and pollution and damage to the environment and the human body can be caused due to the existence of formaldehyde.
In conclusion, by means of the technical scheme, the chemical copper plating solution preparation process is intelligently controlled by constructing the fuzzy controller, real-time monitoring and capturing can be carried out on the change of each parameter in the copper plating solution, and then fuzzy control of automatic addition of each component is carried out by utilizing a fuzzy control rule to carry out feedback, so that an automatic intelligent preparation flow is formed, the preset basic parameters of the chemical copper plating solution are met, and the aims of high-speed response, flexible control and accurate preparation are fulfilled.
The prepared copper sulfate solution is washed by active carbon in advance, so that the purity of the copper sulfate solution can be effectively improved, and the contents of impurities and redundant ions in the copper sulfate solution are reduced and removed, so that the copper plating film coating performance of the copper plating solution is improved; and after the preparation is finished, impurities in the copper plating solution can be effectively removed by cleaning with hydrogen peroxide, so that the solution is maintained and stabilized, and the service life of the copper plating solution is effectively prolonged.
The reducing agent prepared by mixing glyoxylic acid and glyoxylic acid is matched with the additive and the complexing agent quantitatively prepared from ethylenediamine tetraacetic acid and triethanolamine, so that the deposition rate of the copper plating solution can be greatly improved, the efficiency of the copper plating solution is ensured, and meanwhile, the flatness and the brightness of the surface of the PCB can be greatly improved through the surfactant, so that the PCB with uniform, bright and smooth floating layer is formed.
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. An intelligent preparation process of electroless copper plating solution applied to a PCB is characterized by comprising the following steps:
s1, dissolving 30-60 parts of blue vitriod in water, cleaning and filtering to obtain a blue vitriod solution;
s2, sequentially adding 35-50 parts of additive, 40-70 parts of reducing agent, 20-40 parts of complexing agent, 6-15 parts of stabilizer, 8-15 parts of accelerator and 2-5 parts of surfactant into the copper sulfate solution by using an automatic adding instrument, and uniformly stirring to obtain a mixed solution;
s3, adding a proper amount of pH regulator into the mixed solution by using an automatic adding instrument;
s4, measuring parameters of the mixed solution by using monitoring equipment;
s5, controlling parameters of the mixed solution by using a fuzzy controller, and adjusting the operation of each automatic adding instrument until the parameters meet a set value range;
and S6, cleaning the prepared mixed solution by using hydrogen peroxide, and filtering to remove impurities to obtain the final chemical copper plating solution.
2. The intelligent preparation process of the electroless copper plating solution for the PCB as claimed in claim 1, wherein 30-60 parts of blue copperas are dissolved in water for cleaning and filtering to obtain the copper sulfate solution, comprising the following steps:
s11, weighing 30-60 parts of blue copperas, placing in deionized water at 40-60 ℃, and stirring until the blue copperas are completely dissolved;
s12, adding activated carbon into the completely dissolved solution, standing for 10-20h, and filtering;
and S13, adding sulfuric acid into the filtered solution and uniformly stirring to obtain a copper sulfate solution.
3. The intelligent preparation process of the electroless copper plating solution applied to the PCB as claimed in claim 1, wherein the additive comprises at least two of thiourea, 2,2-bipyridine, L-arginine, potassium ferrocyanide;
the complexing agent comprises ethylene diamine tetraacetic acid and triethanolamine, and the mass portion ratio is 1:1.
4. the intelligent preparation process of the electroless copper plating solution applied to the PCB as claimed in claim 1, wherein the reducing agent comprises glyoxylic acid and glyoxylic acid, and the mass part ratio of the glyoxylic acid to the glyoxylic acid is 2:5.
5. the intelligent preparation process of the electroless copper plating solution for the PCB as claimed in claim 1, wherein the stabilizer comprises sodium sulfite and polyoxyethylene sorbitan monostearate, and the mass part ratio is 1:4.
6. the intelligent preparation process of electroless copper plating solution for PCB as claimed in claim 1, wherein the surfactant is tween-80;
the accelerator comprises at least one of aminopyridine, ammonium chloride, nickel sulfate, ferrous sulfate, cytosine, 2-mercaptobenzothiazole, adenine and benzotriazole.
7. The intelligent preparation process of electroless copper plating solution for PCB according to claim 1, wherein the pH adjusting agent comprises sodium hydroxide and sodium carbonate, and the pH value is between 11.8-12.7.
8. The intelligent preparation process of the electroless copper plating solution for the PCB as claimed in claim 1, wherein the monitoring device comprises a temperature sensor, a pH meter probe and a photoelectric colorimeter; the parameters include copper ion concentration, pH and temperature.
9. The intelligent preparation process of electroless copper plating solution for PCB according to claim 1 or 8, wherein the fuzzy controller comprises a database, a knowledge base, a fuzzy control rule set and a fuzzy logic reasoning unit;
the database is used for storing parameters and production data in the preparation process;
the knowledge base is used for storing professional technical knowledge;
the fuzzy control rule set is used for constructing and storing fuzzy control rules to meet the requirements of the preparation process aiming at the characteristics of the change of the electroless copper plating solution;
and the fuzzy logic reasoning unit is used for matching a corresponding fuzzy control rule according to the current parameter and the control state and outputting fuzzy control.
10. The intelligent preparation process of electroless copper plating solution for PCB according to claim 9, wherein the control state comprises:
in the formula (I), the compound is shown in the specification,
representing the characteristic state of the fuzzy controller,
the deviation of the system is indicated by,Ra given value of a parameter is represented,Yindicating the current value of E is added.
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| CN104651814A (en) * | 2014-11-28 | 2015-05-27 | 广东致卓精密金属科技有限公司 | Chemical copper plating solution and chemical copper plating method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104651814A (en) * | 2014-11-28 | 2015-05-27 | 广东致卓精密金属科技有限公司 | Chemical copper plating solution and chemical copper plating method |
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