CN112376095A - Electroplating process for preventing high-temperature tin melting - Google Patents
Electroplating process for preventing high-temperature tin melting Download PDFInfo
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- CN112376095A CN112376095A CN202011267625.6A CN202011267625A CN112376095A CN 112376095 A CN112376095 A CN 112376095A CN 202011267625 A CN202011267625 A CN 202011267625A CN 112376095 A CN112376095 A CN 112376095A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
- C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/30—Electroplating: Baths therefor from solutions of tin
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
- C25D3/40—Electroplating: Baths therefor from solutions of copper from cyanide baths, e.g. with Cu+
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Abstract
The invention relates to the technical field of electroplating processes, in particular to an electroplating process for preventing high-temperature tin melting, which comprises the following steps: putting the base material into electrolyte to remove oil stains; putting the base material without the oil stain into an activating solution for activating treatment; pre-plating copper on the activated base material; carrying out copper plating on the base material which is pre-plated with copper; plating nickel on the base material plated with copper; tin plating is carried out on the base material which is plated with nickel; and putting the substrate which is subjected to tin plating into protective water for tin protection treatment. The invention adds the processes of pre-plating copper and plating copper in the electrotinning process, changes the surface performance of the plating layer of the priming layer, ensures that the tin layer is uniformly distributed on the surface after being cooled at high temperature, solves the problem of tin melting caused by tin flowing and tin accumulation, and meets the market demand.
Description
Technical Field
The invention relates to the technical field of electroplating processes, in particular to an electroplating process for preventing high-temperature tin melting.
Background
Tin is a silver white metal, has high chemical stability, is resistant to oxidation and difficult to discolor in the atmosphere, does not react with sulfide, hardly reacts with sulfuric acid, hydrochloric acid, nitric acid and dilute solutions of some organic acids, and can slowly react by heating even in concentrated hydrochloric acid and dilute sulfuric acid. Because the melting point of tin is 232 ℃, the tin has low melting point, good solderability, good conductivity, difficult color change and good corrosion resistance, a tin layer is often electroplated on the surfaces of electronic components, connecting pieces, leads and printed circuit boards. The existing tin electroplating process is that nickel is directly electroplated after the base material is subjected to oil removal and acid washing treatment, then tin is plated on the surface of a nickel layer, the tin layer flows away from the surface of the nickel layer and exposes out of the nickel layer after being baked at 260 ℃ for 90 seconds, the tin layer can be stacked together, and the tin flowing and tin stacking melting phenomenon can occur on the surface of a workpiece after the tin layer is cooled due to the fact that the surface tension of the tin layer is increased. As shown in fig. 2.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention aims to: the electroplating process for preventing high-temperature tin melting is provided, and the tin layer is uniformly distributed after being cooled at high temperature by changing the surface performance of the bottom coating, so that the tin melting problem of tin flowing and tin accumulation is solved.
In order to achieve the purpose, the invention adopts the following technical scheme:
an electroplating process for preventing high-temperature tin melting comprises the following steps:
putting the base material into electrolyte to remove oil stains;
putting the base material without the oil stain into an activating solution for activating treatment;
pre-plating copper on the activated base material;
carrying out copper plating on the base material which is pre-plated with copper;
plating nickel on the base material plated with copper;
tin plating is carried out on the base material which is plated with nickel;
and putting the substrate which is subjected to tin plating into protective water for tin protection treatment.
Further, in the step of removing oil stains by putting the base material into the electrolyte, putting the base material into the electrolyte for electrolysis for 3-5 minutes, and then cleaning the base material by using tap water; the electrolyte is PT-200 electrolyte, the PT-200 electrolyte contains 90-110 g/L of deoiling powder, the temperature of the PT-200 electrolyte solution is 50-70 ℃, and the current density is 1-5 amperes/square decimeter.
Further, in the step of putting the greasy dirt removed base material into an activating solution for activating treatment, the base material is put into an acid salt solution at room temperature for soaking for 30-60 seconds, then is cleaned by tap water, and then is cleaned by RO water; the acid salt solution contains 75-95 g/L of the salt.
Further, in the step of pre-plating copper on the activated base material, the activated base material is placed into a first plating solution at room temperature for electrodeposition for 1-2 minutes, the current density is 1-5 amperes/square decimeter, and then the pre-plated copper base material is washed by RO water; the first plating solution contains 15-25 g/L copper cyanide and 23-37 g/L potassium cyanide.
Further, in the step of copper plating of the base material which is pre-plated with copper, the base material which is pre-plated with copper is placed into a second plating solution at room temperature for electrodeposition for 5-6 minutes, the current density is 1-5 amperes per square decimeter, so that a copper layer with the thickness of 2 microns is formed on the base material, and then the base material which is plated with copper is cleaned by RO water; the second plating solution contains 40-60 g/L copper cyanide and 30-50 g/L potassium cyanide.
Further, in the step of plating nickel on the copper-plated base material, the copper-plated base material is placed into a third plating solution for electrodeposition for 70-90 seconds, the current density is 1-5 amperes/square decimeter, so that a nickel layer with the thickness of 0.12 microns is formed on the base material, and then the nickel-plated base material is cleaned by RO water; the third plating solution contains 60-80 g/L of nickel sulfamate, 5-15 g/L of nickel chloride and 35-45 g/L of boric acid; the temperature of the third plating solution is 55-65 ℃, and the pH value of the third plating solution is 3.8-4.4.
Further, in the step of carrying out tin plating on the nickel-plated base material, the nickel-plated base material is placed into a fourth plating solution at room temperature for electrodeposition for 15-17 minutes, the current density is 1-5 amperes per square decimeter, so that a tin layer with the thickness of 3.5 microns is formed on the base material, and then the base material after tin plating is cleaned by RO water; the fourth plating solution contains 35-45 g/L of tin methane sulfonate and 170-230 ml/L of SO acid.
Further, in the step of putting the base material which is subjected to tin plating into protective water for tin protection treatment, the base material which is subjected to tin plating is put into the protective water at room temperature for soaking for 20-40 seconds, the protective water is a tin high-temperature discoloration resistant agent solution, and the concentration of the tin high-temperature discoloration resistant agent solution is 20-40%.
In summary, the present invention has the following advantages:
the invention adds the processes of pre-plating copper and plating copper in the electrotinning process, changes the surface performance of the plating layer of the priming layer, ensures that the tin layer is uniformly distributed on the surface after being cooled at high temperature, solves the problem of tin melting caused by tin flowing and tin accumulation, and meets the market demand.
Drawings
FIG. 1 is a schematic diagram of an electroplating process of the present invention.
Fig. 2 is a schematic view of the surface of a tin layer in a conventional electroplating process.
FIG. 3 is a schematic view of the surface of a tin layer under the electroplating process of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and detailed description.
As shown in fig. 1, an electroplating process for preventing high temperature tin melting includes the following steps:
putting the base material into electrolyte to remove oil stains;
putting the base material without the oil stain into an activating solution for activating treatment;
pre-plating copper on the activated base material;
carrying out copper plating on the base material which is pre-plated with copper;
plating nickel on the base material plated with copper;
tin plating is carried out on the base material which is plated with nickel;
and putting the substrate which is subjected to tin plating into protective water for tin protection treatment.
As shown in fig. 1, in the step of removing oil stains by putting the base material into the electrolyte, the base material is put into the electrolyte to be electrolyzed for 3-5 minutes and then cleaned by tap water; the electrolyte is PT-200 electrolyte, the PT-200 electrolyte contains 90-110 g/L of deoiling powder, the temperature of the PT-200 electrolyte solution is 50-70 ℃, and the current density is 1-5 amperes/square decimeter. The base material is subjected to electrolysis to remove oil stains, so that the binding force between the base material and the copper layer can be enhanced.
As shown in fig. 1, in the step of putting the degreased base material into an activation solution for activation treatment, the base material is put into an acid salt solution at room temperature for soaking for 30-60 seconds, then is cleaned by tap water, and is cleaned by RO water; the acid salt solution contains 75-95 g/L of the salt. The base material is activated, so that the oxide on the surface of the base material can be removed, and the bonding force between the base material and the copper layer is enhanced.
As shown in fig. 1, in the step of pre-plating copper on the activated substrate, the activated substrate is placed into a first plating solution at room temperature for electrodeposition for 1 to 2 minutes with a current density of 1 to 5 amperes per square decimeter, and then the pre-plated copper substrate is washed with RO water; the first plating solution contains 15-25 g/L copper cyanide and 23-37 g/L potassium cyanide. The pre-plating of copper on the base material can enhance the binding force between the base material and the copper layer, and the pre-plating is impact plating, and aims to form a very thin compact copper plating layer on the surface of the base material and lay a foundation for the subsequent thick copper plating layer.
As shown in fig. 1, in the step of copper plating the pre-plated copper substrate, the pre-plated copper substrate is placed in a second plating solution at room temperature for electrodeposition for 5 to 6 minutes with a current density of 1 to 5 amperes per square decimeter to form a copper layer with a thickness of 2 μm on the substrate, and then the copper-plated substrate is washed with RO water; the second plating solution contains 40-60 g/L copper cyanide and 30-50 g/L potassium cyanide. The copper layer is plated on the pre-plated copper layer of the base material, so that the tin layer can be effectively prevented from melting tin at high temperature.
As shown in fig. 1, in the step of plating nickel on the copper-plated substrate, the copper-plated substrate is put into a third plating solution for electrodeposition for 70-90 seconds with a current density of 1-5 amperes/square decimeter to form a nickel layer with a thickness of 0.12 μm on the substrate, and then the nickel-plated substrate is washed with RO water; the third plating solution contains 60-80 g/L of nickel sulfamate, 5-15 g/L of nickel chloride and 35-45 g/L of boric acid; the temperature of the third plating solution is 55-65 ℃, and the pH value of the third plating solution is 3.8-4.4. The copper layer of the base material is plated with the nickel layer again, so that the bottom metal can be prevented from entering the tin layer and affecting the performance of the tin layer; the nickel layer is a protective coating which can prevent the mutual influence among coatings after the molecular diffusion.
As shown in fig. 1, in the step of tin plating the nickel-plated substrate, the nickel-plated substrate is placed in a fourth plating solution at room temperature for electrodeposition for 15-17 minutes at a current density of 1-5 ampere/square decimeter to form a tin layer with a thickness of 3.5 μm on the substrate, and then the tin-plated substrate is washed with RO water; the fourth plating solution contains 35-45 g/L of tin methane sulfonate and 170-230 ml/L of SO acid. And plating a tin layer on the nickel layer of the substrate to obtain the functional plating layer.
As shown in fig. 1, in the step of performing tin protection treatment by putting the substrate with tin plating in protection water, the substrate with tin plating is put in protection water at room temperature and soaked for 20 to 40 seconds, the protection water is a tin high temperature discoloration resistant agent solution, and the concentration of the tin high temperature discoloration resistant agent solution is 20 to 40 percent. The tin protection treatment is carried out on the base material which is subjected to tin plating, so that an organic protective film can be formed on the surface of the tin layer, and the oxidation and discoloration of the tin layer are prevented.
As shown in fig. 3, after the tin layer is baked at 260 ℃ for 90S, the tin layer is uniformly distributed on the surface of the nickel layer, and the tin melting phenomenon of tin layer flowing and tin layer accumulation does not occur.
The invention is further illustrated by the following specific examples:
example one
The substrate was first placed in an electrolyte for 3 minutes and then washed with tap water.
The substrate was then immersed in an acid salt solution at room temperature for 30 seconds, then rinsed with tap water and then rinsed with RO water.
And then the activated base material is put into the first plating solution at room temperature for electrodeposition for 1 minute, the current density is 1 ampere/square decimeter, and then the base material which is subjected to the pre-copper plating is washed by RO water.
And then the substrate which is pre-plated with copper is placed into a second plating solution for electrodeposition for 5 minutes at room temperature, the current density is 1 ampere/square decimeter, so that a copper layer with the thickness of 2 mu m is formed on the substrate, and then the substrate after copper plating is cleaned by RO water.
And then the substrate plated with the copper is put into a third plating solution for electrodeposition for 70 seconds, a nickel layer with the thickness of 0.12 mu m is formed on the substrate by adopting the current density of 1 ampere/square decimeter, and then the substrate plated with the nickel is cleaned by RO water.
And then the nickel-plated substrate is put into a fourth plating solution at room temperature for electrodeposition for 15 minutes, a tin layer with the thickness of 3.5 mu m is formed on the substrate by adopting the current density of 1 ampere/square decimeter, and then the tin-plated substrate is cleaned by RO water.
And then the base material which is finished with tin plating is placed into protective water at room temperature for soaking for 20 seconds, the protective water is a tin high-temperature discoloration resistant agent solution, the concentration of the tin high-temperature discoloration resistant agent solution is 20 percent, so that an organic protective film is formed on the surface of the tin layer, and the oxidation and discoloration of the tin layer are prevented.
Example two
The substrate was first placed in an electrolyte for 5 minutes and then washed with tap water.
The substrate was then immersed in an acid salt solution at room temperature for 60 seconds, then rinsed with tap water and then rinsed with RO water.
Then putting the activated base material into the first plating solution at room temperature for electrodeposition for 2 minutes, wherein the current density is 5 amperes/square decimeter, and then washing the base material subjected to the pre-copper plating by using RO water; the first plating solution contained 25g/L of copper cyanide and 37g/L of potassium cyanide.
Then putting the substrate which is pre-plated with copper into a second plating solution at room temperature for electrodeposition for 6 minutes, adopting the current density of 5 amperes/square decimeter to form a copper layer with the thickness of 2 mu m on the substrate, and then washing the substrate which is plated with copper by using RO water; the second plating solution contained 60g/L of copper cyanide and 50g/L of potassium cyanide.
Then putting the copper-plated base material into a third plating solution for electrodeposition for 90 seconds, adopting the current density of 5 amperes/square decimeter to form a nickel layer with the thickness of 0.12 mu m on the base material, and then cleaning the nickel-plated base material by using RO water; the third plating solution contains 80g/L of nickel sulfamate, 15g/L of nickel chloride and 45g/L of boric acid; the temperature of the third plating solution was 65 ℃ and the pH of the third plating solution was 4.4.
Then putting the nickel-plated base material into a fourth plating solution at room temperature for electrodeposition for 17 minutes, adopting a current density of 5 amperes/square decimeter to form a tin layer with the thickness of 3.5 mu m on the base material, and then cleaning the tin-plated base material by using RO water; the fourth plating solution contained 45g/L of tin methanesulfonate and 230ml/L of SO acid.
And then the base material which is finished with tin plating is placed into protective water for soaking for 40 seconds at room temperature, the protective water is a tin high-temperature discoloration resistant agent solution, the concentration of the tin high-temperature discoloration resistant agent solution is 40 percent, so that an organic protective film is formed on the surface of the tin layer, and the oxidation and discoloration of the tin layer are prevented.
EXAMPLE III
The substrate was first placed in an electrolyte for 3 minutes and then washed with tap water.
The substrate was then immersed in an acid salt solution at room temperature for 30 seconds, then rinsed with tap water and then rinsed with RO water.
Then putting the activated base material into the first plating solution at room temperature for electrodeposition for 1 minute, wherein the current density is 1 ampere/square decimeter, and then washing the base material subjected to pre-copper plating by using RO water; the first plating solution contains 15g/L of copper cyanide and 23g/L of potassium cyanide.
Then putting the substrate which is pre-plated with copper into a second plating solution at room temperature for electrodeposition for 5 minutes, adopting the current density of 1 ampere/square decimeter to form a copper layer with the thickness of 2 mu m on the substrate, and then washing the substrate which is plated with copper by using RO water; the second plating solution contained 40g/L of copper cyanide and 30g/L of potassium cyanide.
Then putting the copper-plated base material into a third plating solution for electrodeposition for 70 seconds, adopting the current density of 1 ampere/square decimeter to form a nickel layer with the thickness of 0.12 mu m on the base material, and then cleaning the nickel-plated base material by using RO water; the third plating solution contains 60g/L of nickel sulfamate, 5g/L of chloride nickel and 35g/L of boric acid; the temperature of the third plating solution was 55 ℃ and the pH of the third plating solution was 3.8.
Then putting the nickel-plated base material into a fourth plating solution at room temperature for electrodeposition for 15 minutes, adopting a current density of 1 ampere/square decimeter to form a tin layer with the thickness of 3.5 mu m on the base material, and then cleaning the tin-plated base material by using RO water; the fourth plating solution contained 35g/L of tin methanesulfonate and 170ml/L of SO acid.
And then the substrate after the tin plating is finished is placed into protective water at room temperature for soaking for 20 seconds, wherein the protective water is a tin high-temperature discoloration resistant agent solution, and the concentration of the tin high-temperature discoloration resistant agent solution is 20%. So as to form an organic protective film on the surface of the tin layer to prevent the oxidation and discoloration of the tin layer.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, but the embodiments of the present invention are not limited by the above-mentioned embodiments, and any other changes, modifications, substitutions, combinations, simplifications which do not depart from the spirit and principle of the present invention should be regarded as equivalent substitutions, and all are included in the scope of the present invention.
Claims (8)
1. An electroplating process for preventing high-temperature tin melting is characterized in that: the method comprises the following steps:
putting the base material into electrolyte to remove oil stains;
putting the base material without the oil stain into an activating solution for activating treatment;
pre-plating copper on the activated base material;
carrying out copper plating on the base material which is pre-plated with copper;
plating nickel on the base material plated with copper;
tin plating is carried out on the base material which is plated with nickel;
and putting the substrate which is subjected to tin plating into protective water for tin protection treatment.
2. An electroplating process for preventing high temperature tin melting according to claim 1, wherein: in the step of removing oil stains by putting the base material into electrolyte, putting the base material into the electrolyte for electrolysis for 3-5 minutes, and then cleaning the base material by using tap water; the electrolyte is PT-200 electrolyte, the PT-200 electrolyte contains 90-110 g/L of deoiling powder, the temperature of the PT-200 electrolyte solution is 50-70 ℃, and the current density is 1-5 amperes/square decimeter.
3. An electroplating process for preventing high temperature tin melting according to claim 1, wherein: in the step of putting the base material without the oil stain into an activating solution for activating treatment, putting the base material into an acid salt solution at room temperature for soaking for 30-60 seconds, then washing with tap water, and then washing with RO water; the acid salt solution contains 75-95 g/L of the salt.
4. An electroplating process for preventing high temperature tin melting according to claim 1, wherein: in the step of pre-plating copper on the base material after activation treatment, the base material after activation treatment is placed into a first plating solution at room temperature for electrodeposition for 1-2 minutes, the current density is 1-5 amperes/square decimeter, and then the base material after pre-plating copper is cleaned by RO water; the first plating solution contains 15-25 g/L copper cyanide and 23-37 g/L potassium cyanide.
5. An electroplating process for preventing high temperature tin melting according to claim 1, wherein: in the step of copper plating of the base material which is pre-plated with copper, the base material which is pre-plated with copper is placed into a second plating solution at room temperature for electrodeposition for 5-6 minutes, the current density is 1-5 amperes per square decimeter, so that a copper layer with the thickness of 2 microns is formed on the base material, and then the base material which is plated with copper is cleaned by RO water; the second plating solution contains 40-60 g/L copper cyanide and 30-50 g/L potassium cyanide.
6. An electroplating process for preventing high temperature tin melting according to claim 1, wherein: in the step of plating nickel on the copper-plated base material, the copper-plated base material is placed into a third plating solution for electrodeposition for 70-90 seconds, the current density is 1-5 amperes/square decimeter, so that a nickel layer with the thickness of 0.12 microns is formed on the base material, and then the nickel-plated base material is cleaned by RO water; the third plating solution contains 60-80 g/L of nickel sulfamate, 5-15 g/L of nickel chloride and 35-45 g/L of boric acid; the temperature of the third plating solution is 55-65 ℃, and the pH value of the third plating solution is 3.8-4.4.
7. An electroplating process for preventing high temperature tin melting according to claim 1, wherein: in the step of carrying out tin plating on the nickel-plated base material, putting the nickel-plated base material into a fourth plating solution at room temperature for electrodeposition for 15-17 minutes, adopting a current density of 1-5 amperes/square decimeter to form a tin layer with the thickness of 3.5 micrometers on the base material, and then washing the tin-plated base material with RO water; the fourth plating solution contains 35-45 g/L of tin methane sulfonate and 170-230 ml/L of SO acid.
8. An electroplating process for preventing high temperature tin melting according to claim 1, wherein: in the step of putting the base material which is finished with tin plating into protective water for tin protection treatment, the base material which is finished with tin plating is put into the protective water at room temperature for soaking for 20-40 seconds, the protective water is a tin high-temperature discoloration resistant agent solution, and the concentration of the tin high-temperature discoloration resistant agent solution is 20% -40%.
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