CN111945139B - Nickel plating method for copper-clad ceramic substrate - Google Patents
Nickel plating method for copper-clad ceramic substrate Download PDFInfo
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- CN111945139B CN111945139B CN202010730421.5A CN202010730421A CN111945139B CN 111945139 B CN111945139 B CN 111945139B CN 202010730421 A CN202010730421 A CN 202010730421A CN 111945139 B CN111945139 B CN 111945139B
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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
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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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
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1837—Multistep pretreatment
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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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/18—Acidic compositions for etching copper or alloys thereof
-
- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F3/00—Brightening metals by chemical means
- C23F3/04—Heavy metals
- C23F3/06—Heavy metals with acidic solutions
Abstract
The invention relates to a nickel plating method for a copper-clad ceramic substrate, which is carried out after the patterning process of a ceramic copper-clad plate and comprises the following steps: 1) preparing a high-gloss copper surface: under the condition of 20-35 ℃, putting the copper-clad ceramic substrate into polishing solution for polishing for 5-30 min, and keeping the state of a wet plate without drying after polishing; 2) cleaning and drying: sequentially carrying out oil removal, acid microetching, overflow water washing, cold air blow-drying, anti-oxidation cleaning, overflow water washing and ultrasonic water washing on the copper-clad ceramic substrate treated in the step 1), firstly carrying out surface water absorption treatment, and then drying by adopting hot air; 3) chemical nickel plating: and (3) carrying out weak etching, water washing, activation and water washing on the copper-clad ceramic substrate treated in the step 2) in sequence, and then carrying out chemical nickel plating. The chemical nickel plating uses the chemical nickel plating solution of nickel sulfate and sodium hypophosphite system, the pH value is controlled to be 4-6 during nickel plating, and the temperature is controlled to be 80-100 ℃.
Description
Technical Field
The invention belongs to the technical field of semiconductor substrate preparation, relates to a preparation technology for improving the weldability of a copper-clad ceramic substrate, and particularly relates to a nickel plating method for obtaining a copper-clad ceramic substrate with a bright uniform high-gloss nickel plating layer.
Background
The IGBT module is a modularized semiconductor product formed by bridge packaging of an IGBT (insulated gate bipolar transistor chip) and an FWD (freewheeling diode chip) through a specific circuit; copper-clad ceramic substrates are widely used as a substrate in IGBT modules. In the packaging process of the IGBT power module, the IGBT/FRD chip, the terminal, the lining plate and the substrate are connected together by welding, the rework rate and the qualification rate of the module are directly influenced by the quality of the welding process, and the welding quality is directly related to the reliability of the module. Welding generally employs a two-step process: firstly, welding a ceramic copper-clad plate and a chip; and secondly, welding the chip terminal and the ceramic copper clad plate and welding the ceramic copper clad plate and the aluminum substrate. The ceramic copper-clad plate is required to have good weldability to ensure the welding quality.
The nickel plating of the ceramic copper clad laminate is an effective mode for improving the weldability of the substrate, the nickel electroplating is difficult and the obtained plating layer is uneven aiming at the patterned copper clad laminate, and the chemical nickel plating is an effective mode for obtaining a good nickel plating layer. The bright and uniform high-gloss nickel plating layer is one of the prerequisites for preparing the copper-clad ceramic substrate with excellent welding performance and high quality (compact plating layer, corrosion resistance and the like).
In order to solve the above problems, the prior art has conducted many beneficial researches, such as patents CN1203211C and CN105648480A and journal "brief description of high-uniformity bright nickel plating method", which all mention the methods for obtaining bright and uniform high-surface nickel plating layer, mainly including: 1) adding a brightening agent into the chemical nickel plating solution; 2) bright nickel electroplating is carried out after chemical nickel plating; 3) and after nickel plating, polishing to obtain a high-gloss surface coating.
However, if the method is applied to the nickel plating of the copper-clad ceramic substrate, the defects are obvious: the method 2) is not suitable for a patterned copper-clad plate; the addition of the brightener in the method 1) can cause the change of the plating speed, meanwhile, the addition of the brightener also brings great difficulty to the control of process parameters, and the residual brightener can cause the deterioration of weldability; the polishing procedure in the method 3) is complicated, and the nickel coating of the copper-clad plate with the thickness of 2-20 mu m is difficult and high in cost no matter the polishing is carried out by chemical electrolyte or physical polishing.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides the nickel plating method for the copper-clad ceramic substrate to obtain the bright and uniform high-gloss nickel plating layer, the method is simple and easy to implement, low in cost and wide in applicability, and the weldability of the metal ceramic substrate can be obviously improved.
The invention abandons the traditional mode of improving the nickel plating solution or the nickel plating layer, and has the technical key that the copper-clad ceramic substrate of the high-gloss copper is prepared firstly, and then nickel is plated on the high-gloss copper, thereby realizing the high-gloss nickel plating. In addition, the weldability of the nickel plating layer can be obviously improved by cleaning the nickel plating layer with an organic solvent under the ultrasonic condition. In order to achieve the purpose, the invention is implemented by the following technical scheme:
the nickel plating method of the copper-clad ceramic substrate provided by the invention is carried out after the patterning process of the ceramic copper-clad plate, and comprises the following steps: 1) preparing a high-gloss copper surface: under the condition of 20-35 ℃, putting the copper-clad ceramic substrate into polishing solution for polishing for 5-30 min, and keeping the state of a wet plate without drying after polishing; 2) cleaning and drying: sequentially carrying out oil removal, acid microetching, overflow water washing, cold air blow-drying, anti-oxidation cleaning, overflow water washing and ultrasonic water washing on the copper-clad ceramic substrate treated in the step 1), firstly carrying out surface water absorption treatment, and then drying by adopting hot air; 3) chemical nickel plating: and (3) carrying out weak etching, water washing, activation and water washing on the copper-clad ceramic substrate treated in the step 2) in sequence, and then carrying out chemical nickel plating. The chemical nickel plating uses the chemical nickel plating solution of nickel sulfate and sodium hypophosphite system, the pH value is controlled to be 4-6 during nickel plating, and the temperature is controlled to be 80-100 ℃.
Preferably, the method for plating nickel on the copper-clad ceramic substrate further comprises an ultrasonic solvent cleaning step, wherein the copper-clad ceramic substrate after nickel plating is immersed in one or more of absolute ethyl alcohol, isopropanol and acetone, and is subjected to ultrasonic treatment at normal temperature for 15-30 min, and then is subjected to water washing and drying. Preferably, the water washing is normal-temperature pure water ultrasonic washing for 5min-10min, and the drying is 80-100 ℃ hot air drying for 5min-30 min.
Tests prove that the weldability of the nickel-plated copper-clad ceramic substrate is further improved by cleaning the nickel-plated copper-clad ceramic substrate with the ultrasonic solvent.
Preferably, in the nickel plating method for the copper-clad ceramic substrate provided by the invention, in the step 1), a sodium chlorate and hydrochloric acid system polishing solution is selected as the polishing solution, and in the polishing solution, the concentration of sodium chlorate is 1.0-1.3g/L, and the concentration of hydrochloric acid is 20g/L-80 g/L.
Preferably, in the nickel plating method for the copper-clad ceramic substrate provided by the invention, in the step 2), during oil removal treatment, the copper-clad ceramic substrate is sequentially subjected to ultrasonic immersion cleaning in an acetone solution for 3min to 5min, in absolute ethyl alcohol for 1min to 3min and in pure water for 1min to 3 min; when in acid microetching treatment, the treatment is carried out for 3-5min by acid etching solution containing 2-4g/L sulfuric acid and 40-80g/L sodium thiosulfate at the temperature of 20-40 ℃; the conditions of the two times of overflow water washing are normal-temperature overflow water washing for 1-5 min; the drying temperature of the cold air is 15-25 ℃, and the treatment time is 3-10 min; during anti-oxidation cleaning, a copper surface antioxidant commonly used in the field is adopted for treatment for 1-5 min; and when ultrasonic washing is carried out, normal-temperature pure water is adopted for ultrasonic washing for 5-10 min.
Preferably, in the nickel plating method for the copper-clad ceramic substrate provided by the invention, in the step 2), the washed copper-clad ceramic substrate is dried by a water absorption roller, and then dried under the condition of hot air at 80-100 ℃.
Preferably, in the nickel plating method for the copper-clad ceramic substrate provided by the invention, in the step 3), dilute sulfuric acid of 5-50g/L is adopted for room temperature treatment for 5-15 s during weak etching treatment; when water washing treatment is carried out, washing with water at normal temperature for 60-150 s; during the activation treatment, ionic palladium salt activating solution is used, the activation temperature is 15-30 ℃, and the activation time is 60-200 s; preferably, in the nickel plating method for the copper-clad ceramic substrate, the content of nickel sulfate in the chemical nickel plating solution is 10-25g/L, the content of sodium hypophosphite is 15-20g/L, and the pH value of the solution is controlled to be 4.9-5.3.
The invention has the following beneficial effects:
the invention abandons the traditional mode of improving nickel plating solution or nickel plating layer, firstly prepares the high-gloss copper surface, cleans and dries the copper surface, and then carries out chemical nickel plating to realize the high-gloss nickel plating, and the technical effects are as follows: 1) because the chemical polishing of the copper layer is used for replacing the polishing of the nickel layer, the copper layer is thicker (>0.2mm) and the nickel layer is thinner (2-20 mu m), and the copper layer polishing is easy to operate and control, compared with the chemical nickel plating brightener, the chemical nickel plating process is more stable and controllable; 2) the invention can be compounded with the existing high-gloss surface nickel plating technology, the method has wide applicability, and can be used for preparing copper-clad ceramic substrates by aiming at various processes; 3) the method is simple and practical, low in cost and good in effect.
Drawings
FIG. 1 is a flowchart of a nickel plating method for a copper-clad ceramic substrate according to example 1 of the present invention;
fig. 2 is a flowchart of a nickel plating method for a copper-clad ceramic substrate in embodiment 2 of the present invention.
Detailed Description
The following embodiments are implemented on the premise of the technical scheme of the present invention, and give detailed implementation modes and specific operation procedures, but the protection scope of the present invention is not limited to the following embodiments.
The reagents and starting materials used in the present invention are commercially available or can be prepared according to literature procedures. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out according to conventional conditions or according to conditions recommended by the manufacturers.
Example 1
Referring to fig. 1, this embodiment is an implementation process of the nickel plating method for a copper-clad ceramic substrate of the present invention, and sequentially includes the following steps:
1) graphic process for ceramic copper-clad plate
Like the prior art, the copper-clad ceramic substrate for active soldering also comprises solder etching, such as film pasting, exposure, development and copper etching.
2) Preparing high-gloss copper surface
And (3) under the condition of 20-35 ℃, polishing the copper-clad ceramic substrate in a sodium chlorate and hydrochloric acid system polishing solution for 5-30 min, and keeping the state of a wet plate without drying after polishing. In the polishing solution, the concentration of sodium chlorate is 1.0-1.3g/L, and the concentration of hydrochloric acid is 20-80 g/L, preferably 50 g/L.
3) Cleaning and drying
Sequentially carrying out oil removal, acid microetching, overflow water washing, cold air blow-drying, anti-oxidation cleaning, overflow water washing and ultrasonic water washing on the copper-clad ceramic substrate treated in the step 2), carrying out surface water absorption treatment, and then drying by adopting hot air, thereby being a pretreatment process before nickel plating.
When the oil removal treatment is carried out, the copper-clad ceramic substrate is sequentially subjected to ultrasonic immersion cleaning in an acetone solution for 3min to 5min, in absolute ethyl alcohol for 1min to 3min and in pure water for 1min to 3 min; when in acid microetching treatment, the treatment is carried out for 3-5min by acid etching solution containing 2-4g/L sulfuric acid and 40-80g/L sodium thiosulfate at the temperature of 20-40 ℃; when ultrasonic washing is carried out, normal-temperature pure water is adopted for ultrasonic washing for 5-10 min; the overflow washing condition of each time is normal temperature overflow washing for 1-5 min; the drying temperature of cold air is 15-25 ℃, and the treatment time is 3-10 min; during anti-oxidation cleaning, a copper surface antioxidant commonly used in the field is adopted for treatment for 1-5 min; the surface water absorption treatment is to absorb the surface water through a water absorption roller and then dry the surface water under the condition of hot air at 80-100 ℃.
4) Electroless nickel plating
And 3) carrying out weak etching, water washing, activation and water washing on the copper-clad ceramic substrate treated in the step 3) in sequence, and then carrying out chemical nickel plating. The chemical nickel plating uses the chemical nickel plating solution of nickel sulfate and sodium hypophosphite system, the pH value is controlled to be 4-6 during nickel plating, and the temperature is controlled to be 80-100 ℃.
When in weak etching treatment, dilute sulphuric acid of 5-50g/L is adopted for treatment for 5-15 s at room temperature; when water washing treatment is carried out, washing with water at normal temperature for 60-150 s; during the activation treatment, ionic palladium salt activating solution is used, the activation temperature is 15-30 ℃, and the activation time is 60-200 s; the content of nickel sulfate in the chemical nickel plating solution is 10-25g/L, the content of sodium hypophosphite is 15-20g/L, and the pH value of the solution is controlled to be 4.9-5.3.
According to the method, the uniform nickel plating of the copper-clad ceramic substrate can be effectively realized.
Example 2
The embodiment is further optimized by the embodiment 1, and an ultrasonic solvent cleaning process for the copper-clad plate product is added after the step 4) of the embodiment 1, specifically, a sample is immersed in one or a mixture of several solvents of absolute ethyl alcohol, isopropanol and acetone for normal-temperature ultrasonic cleaning for 15min to 30min, then the sample is subjected to ultrasonic cleaning for 5min to 10min by pure water at normal temperature, and is dried for 5min to 30min by hot air at 80 ℃ to 100 ℃.
Example 3
This example is a method for testing the solderability of the copper clad laminate after nickel plating, using a vacuum heating furnace in H2:N2Under the condition that the proportion is 100 percent to 0, the copper clad laminate adhered with the soldering lug (the components are Sn/Ag3.5/Cu0.5+ Ni and Ge) is heated to 300 +/-10 ℃ at a certain heating rate and is kept for 260s at the temperature, and the area of the tin is required to be larger than 95 percent of the area of the soldering lug by visual observation. The test results show examples2 have higher solderability.
While the preferred embodiments of the present invention have been described in detail, it will be understood by those skilled in the art that the invention is not limited thereto, and that various changes and modifications may be made without departing from the spirit of the invention, and the scope of the appended claims is to be accorded the full scope of the invention.
Claims (5)
1. A nickel plating method for a copper-clad ceramic substrate is characterized by being carried out after a patterning process of a ceramic copper-clad plate, and comprises the following steps:
1) preparing high-gloss copper surface
Under the condition of 20-35 ℃, putting the copper-clad ceramic substrate into polishing solution for polishing for 5-30 min, and keeping the state of a wet plate without drying after polishing; the polishing solution is a sodium chlorate and hydrochloric acid system polishing solution, wherein the concentration of sodium chlorate is 1.0-1.3g/L, and the concentration of hydrochloric acid is 20-80 g/L;
2) cleaning and drying
Sequentially carrying out oil removal, acid microetching, overflow water washing, cold air blow-drying, anti-oxidation cleaning, overflow water washing and ultrasonic water washing on the copper-clad ceramic substrate treated in the step 1), firstly carrying out surface water absorption treatment, and then drying by adopting hot air;
3) electroless nickel plating
Sequentially carrying out weak etching, water washing, activation and water washing on the copper-clad ceramic substrate processed in the step 2), and then carrying out chemical nickel plating, wherein the chemical nickel plating uses a chemical nickel plating solution of a nickel sulfate and sodium hypophosphite system, the pH value is controlled to be 4-6 during nickel plating, the temperature is controlled to be 80-100 ℃,
the content of nickel sulfate in the chemical nickel plating solution is 10-25g/L, the content of sodium hypophosphite is 15-20g/L, and the pH value of the solution is controlled to be 4.9-5.3;
4) ultrasonic solvent cleaning
Immersing the nickel-plated copper-clad ceramic substrate in one or more of absolute ethyl alcohol, isopropanol and acetone, carrying out ultrasonic treatment at normal temperature for 15-30 min, and then washing and drying.
2. The nickel plating method for the copper-clad ceramic substrate according to claim 1, characterized in that:
wherein the water washing is normal temperature pure water ultrasonic cleaning for 5min-10min, and drying is 80-100 ℃ hot air drying for 5min-30 min.
3. The nickel plating method for the copper-clad ceramic substrate according to claim 1, characterized in that:
wherein, in the step 2), during oil removal treatment, the copper-clad ceramic substrate is sequentially subjected to ultrasonic immersion cleaning in an acetone solution for 3min to 5min, in absolute ethyl alcohol for 1min to 3min, and in pure water for 1min to 3 min; when in acid microetching treatment, the treatment is carried out for 3-5min by acid etching solution containing 2-4g/L sulfuric acid and 40-80g/L sodium thiosulfate at the temperature of 20-40 ℃; the conditions of the two times of overflow water washing are normal-temperature overflow water washing for 1-5 min; the drying temperature of the cold air is 15-25 ℃, and the treatment time is 3-10 min; during anti-oxidation cleaning, a copper surface antioxidant is adopted for treatment for 1-5 min; and when ultrasonic washing is carried out, normal-temperature pure water is adopted for ultrasonic washing for 5-10 min.
4. The nickel plating method for the copper-clad ceramic substrate according to claim 1, characterized in that:
in the step 2), the washed copper-clad ceramic substrate is dried by a water absorption roller, and then dried under the condition of hot air at 80-100 ℃.
5. The nickel plating method for the copper-clad ceramic substrate according to claim 1, characterized in that:
wherein, in the step 3), dilute sulfuric acid of 5-50g/L is adopted for weak etching treatment, and the treatment is carried out for 5-15 s at room temperature; when water washing treatment is carried out, washing with water at normal temperature for 60-150 s; during the activation treatment, ionic palladium salt activating solution is used, the activation temperature is 15-30 ℃, and the activation time is 60-200 s.
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| CN113471081B (en) * | 2021-06-17 | 2022-10-11 | 江苏富乐华半导体科技股份有限公司 | Method for improving poor appearance of ceramic copper-clad carrier plate after high-temperature sintering |
| CN113799002B (en) * | 2021-08-24 | 2022-07-19 | 江苏富乐华半导体科技股份有限公司 | Copper sheet surface treatment method |
| CN116288289B (en) * | 2023-02-24 | 2023-09-12 | 江苏富乐华半导体科技股份有限公司 | Method for plating nickel and silver on ceramic copper-clad carrier plate |
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