CN111364030A - Pretreatment method for improving flatness of electroless NiP plating layer on aluminum substrate - Google Patents

Pretreatment method for improving flatness of electroless NiP plating layer on aluminum substrate Download PDF

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CN111364030A
CN111364030A CN202010267177.3A CN202010267177A CN111364030A CN 111364030 A CN111364030 A CN 111364030A CN 202010267177 A CN202010267177 A CN 202010267177A CN 111364030 A CN111364030 A CN 111364030A
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aluminum substrate
zinc
solution
plating layer
flatness
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杭弢
周天燊
甘伟星
李明
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Shanghai Jiaotong University
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Shanghai Jiaotong University
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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
    • C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
    • 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
    • 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
    • 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
    • C23C18/52—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 using reducing agents for coating with metallic material not provided for in a single one of groups C23C18/32 - C23C18/50

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemically Coating (AREA)

Abstract

The invention belongs to the technical field of electronic packaging materials, and discloses a pretreatment method for improving the flatness of a chemical plating NiP coating on an aluminum substrate2+In the acid solution, a layer of very thin copper is deposited on the surface of the NiP coating to form an active point during zinc dipping, and then secondary zinc dipping is carried out to form a uniform and fine zinc layer on the surface of the substrate, so that the NiP coating with obviously improved flatness is obtained after chemical plating, and the NiP coating has the advantages of simple process, low cost, mild reaction conditions and the like.

Description

Pretreatment method for improving flatness of electroless NiP plating layer on aluminum substrate
Technical Field
The invention belongs to the technical field of electronic packaging materials, and relates to a pretreatment method for improving the smoothness of an electroless NiP plating layer of an aluminum substrate.
Background
The NiP coating as a diffusion barrier layer can prevent Al and Si from generating interface reaction, and is widely applied to the field of electronic packaging interconnection so as to improve the interface reliability of Al and Si. As interconnect dimensions decrease, the thickness of the NiP diffusion barrier also gradually decreases. In the existing method, the uniformity of the thin NiP coating cannot be ensured because the electroplated NiP coating is easily influenced by the distribution of an electric field; the chemical plating NiP coating is not influenced by an electric field, and can keep thickness uniformity in a plane and a Through Silicon Via (TSV), so that the chemical plating NiP coating is widely applied to the field of advanced electronic packaging at present.
The through silicon via (tsv) packaging technology is a hot spot technology currently applied to packaging products such as CMOS Image Sensors (CIS) and memories. With the trend of miniaturization of microelectronic products, metal layers in TSV are thinner and thinner, and the requirement on uniformity of a diffusion barrier layer is high. At present, most of barrier layers of TSV applied to CIS are deposited on an Al substrate, but when a diffusion barrier layer is prepared on Al by adopting an electroplating method, the current density on the surface of the TSV is not uniformly distributed due to the complex structure of the TSV, and the situations of non-uniform plating and poor smoothness easily occur. Aiming at the problems, the invention adopts chemical plating to replace electroplating to deposit the NiP plating layer on the plane Al. However, since all Al alloys are very susceptible to the formation of transient oxide layers and the oxides are very stable, pretreatment of the base Al prior to electroless plating is necessary. Pretreatment before chemical plating has important influence on the surface state, the binding force, the corrosion resistance and the like of the chemical plating NiP coating. At present, the zinc dipping method is the pretreatment method of the NiP coating of the aluminum-based chemical plating with the most extensive application and very low cost.
In the zincate pretreatment, the surface of the Al substrate is coated with a thin layer of zinc by replacing aluminum with zinc. In the chemical plating process, the zinc layer can prevent the oxide film from regenerating, and finally a uniform and compact NiP plating layer is formed. The pretreatment by the zinc dipping method has the advantages of low cost, simple and convenient operation, simple components of the zinc dipping solution and the like. Thurlow et al, studied in 1989, found that the properties of the zinc layer can greatly affect the electroless plating process that follows and the quality of the electroless plating. The zinc dipping liquid composition, the zinc dipping time, the zinc dipping process, the alloy composition and the like can influence the quality of the zinc layer. The zinc on the aluminum substrate is dissolved during the initial period of electroless plating after the zincing. However, zinc is not only reacted and diffused during the electroless plating process, but zinc ions are also deposited together with nickel after being reduced by a reducing agent. Therefore, to control the initial deposition state of the electroless NiP plating, it is necessary to obtain an excellent zinced surface on the Al substrate.
The pretreatment research of electroless NiP mainly focuses on the research of a substrate, a zinc dipping mode and a zinc dipping solution, and no newly developed pretreatment method exists. The invention adopts Cu2+/H+The pretreatment of the chemical NiP plating layer can obviously improve the smoothness of the chemical NiP plating layer.
Disclosure of Invention
The invention provides a pretreatment method for improving the flatness of an electroless NiP plating layer of an aluminum substrate in order to improve the flatness of the electroless NiP plating layer.
The technical scheme of the invention is as follows:
a pretreatment method for improving the flatness of an electroless NiP plating layer of an aluminum substrate comprises the following steps:
(1) selecting an aluminum substrate material, and carrying out oil removal and acid pickling pretreatment on the aluminum substrate material to clean the surface of the aluminum substrate material;
(2) then dipping it into Cu2+In an acidic solution to deposit copper on the surface thereof, wherein the Cu is contained2+In an acidic solution of Cu2+Has a solubility of 0.5 × 10-3～2×10-3mol/L，H+The concentration of the (A) is 5.0-15.0 mol/L, the temperature is 20-80 ℃, and the time is 30-50 s;
(3) soaking the substrate in a zinc soaking solution for secondary zinc soaking, wherein the zinc soaking solution is a mixed solution of NaOH and ZnO; and finally, carrying out chemical plating to obtain a NiP plating layer on the aluminum substrate.
In an embodiment of the present invention, the aluminum substrate material is pure aluminum or an aluminum alloy.
In one embodiment of the present invention, the acid washing solution has a solubility of 5 to 15 wt% hydrochloric acid.
In one embodiment of the present invention, in the step (3), the concentration of NaOH in the zinc dipping solution is 5 to 20 wt%, and the concentration of ZnO in the zinc dipping solution is 0.1 to 5.0 wt%.
In one embodiment of the invention, in the step (3), the zinc dipping temperature is 20-30 ℃, and the zinc dipping time is 10-60 s.
In one embodiment of the present invention, in the step (3), the dezincing solution is HNO3The concentration of the solution is 20-60 wt%.
In one embodiment of the invention, in the step (3), the zinc removing temperature is 20-30 ℃, and the zinc removing time is 5-30 s.
Compared with the prior art, the invention has the following beneficial effects:
the invention relates to a pretreatment method for improving the flatness of a chemical plating NiP coating on an aluminum substrate, which comprises the steps of firstly carrying out pretreatment such as oil removal, acid washing and the like on the surface of the aluminum substrate, and then immersing the aluminum substrate into Cu-containing2+In the acid solution, a layer of very thin copper is deposited on the surface of the NiP coating to form an active point during zinc dipping, and then secondary zinc dipping is carried out to form a uniform and fine zinc layer on the surface of the substrate, so that the NiP coating with obviously improved flatness is obtained after chemical plating, and the NiP coating has the advantages of simple process, low cost, mild reaction conditions and the like.
Scanning the example 1 and the comparative examples 1-2 by using a scanning electron microscope respectively to obtain an enlarged morphology image of the surface of the aluminum substrate, wherein the morphology image comprises a zinc layer and a NiP coating, as shown in FIG. 2, the roughness of the NiP coating prepared in the example 1 is only 1/4 of the roughness of the NiP coating corresponding to the comparative example 1, and the root-mean-square roughness of the NiP coating is only 5.5 nm. In addition, the concentration was also adjusted to 3.5 wt% NaCl solution and 0.5mol/L H2SO4The solution was tested for corrosion resistance and as shown in fig. 3, the results of the impedance fit analysis showed: through Cu2+/H+The NiP coating after treatment was the most dense. Thus, via Cu2+/H+And (2) treating, namely obtaining a NiP coating with a smoother surface and lower porosity by improving the uniformity of the size and distribution of zinc particles, so that the corrosion resistance of the NiP coating is improved, and the possible principle is as follows: cu2+/H+The thin copper layer after solution treatment can be used as an active point of Zn, which is beneficial to obtaining a smoother Zn layer, and further influences the growth of Ni in the laminated direction, so that the surface smoothness of the NiP coating is greatly improved, and the growth schematic diagrams of the NiP coatings of the embodiment 1 and the comparative example 1 are shown in FIG. 4.
Drawings
FIG. 1 is a flow chart of a pretreatment method for improving the flatness of an electroless NiP plating layer on an aluminum substrate in accordance with example 1 of the present invention;
FIG. 2 is SEM images of the zinc layers and electroless NiP coatings of examples 1 and comparative examples 1-2, wherein a-c are SEM images of the zinc layers of comparative example 1, comparative example 2 and example 1, respectively, and d-f are SEM images of the electroless NiP coatings of comparative example 1, comparative example 2 and example 1, respectively;
FIG. 3 shows the neutralization of electroless NiP plating layers of example 1 and comparative examples 1-2 in 3.5 wt% NaCl solution to 0.5mol/LH2SO4Tafel curves in solution, wherein a to c are Tafel curves of comparative example 1, comparative example 2 and example 1, respectively;
FIG. 4 is a schematic illustration of the NiP plating growth of example 1 and comparative example 1.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are only for illustrating the present invention and are not intended to limit the scope of the present invention. In practice, the invention will be understood to cover all modifications and variations of this invention provided they come within the scope of the appended claims.
For a better illustration of the invention, the following detailed description of the invention is given in conjunction with the accompanying drawings.
Example 1
Referring to fig. 1, a pretreatment method for improving the flatness of an electroless Nickel (NiP) plating layer on an aluminum substrate according to embodiment 1 of the present invention comprises the following steps:
(1) selecting pure aluminum foil with the thickness of 200 microns as an aluminum substrate, and performing oil removal treatment on the aluminum substrate, wherein the oil removal current is 4ASD (A/dm)2) The time is about 10s, and the temperature is controlled at 50 ℃; washing with deionized water, and washing with 10 wt% hydrochloric acid solution for 30 s;
(2) immersing an aluminum substrate in Cu2+The concentration is 1.0 × 10-3mol/L，H+Treating the mixture for 40s at 70 ℃ in a solution with the concentration of 10 mol/L;
(3) at room temperature, an aluminum substrate is immersed into a zinc immersion solution with NaOH solubility of 10 wt% and ZnO solubility of 1.0 wt%, the solution is kept for 10s, then concentrated nitric acid with concentration of 50 wt% is used for treating for 30s, a zinc layer on the surface of the substrate is removed, the substrate is immersed into the zinc immersion solution again for 10s, and finally, chemical plating is carried out under certain conditions (pH 4.880 ℃/0.5h) to obtain a flat NiP plating layer.
Comparative example 1
(1) Selecting pure aluminum foil with the thickness of 200 microns as an aluminum substrate, and performing oil removal treatment on the aluminum substrate, wherein the oil removal current is 4ASD (A/dm)2) The time is about 10s, and the temperature is controlled at 50 ℃; washing with deionized water, and washing with 10 wt% hydrochloric acid solution for 30 s;
(2) at room temperature, an aluminum substrate is immersed in a zinc immersion solution with NaOH solubility of 10 wt% and ZnO solubility of 1.0 wt%, the solution is kept for 30s, then concentrated nitric acid with concentration of 50 wt% is used for treating for 6s, a zinc layer on the surface of the substrate is removed, the substrate is immersed in the zinc immersion solution for 30s, and finally, chemical plating is carried out under certain conditions (pH 4.880 ℃/0.5h) to obtain a flat NiP plating layer.
Comparative example 2
(1) Preferably, a pure aluminum foil with a thickness of 200 microns is selected as an aluminum substrate, and the substrate is subjected to oil removal treatment, wherein the oil removal current is 4ASD (A/dm)2) The time is about 10s, and the temperature is controlled at 50 ℃; washing with deionized water, and washing with 10 wt% hydrochloric acid solution for 30 s;
(2) placing the aluminum substrate in H+Treating in 10mol/L acid solution at 70 deg.C for 40 s;
(3) at room temperature, an aluminum substrate is immersed into a zinc immersion solution with NaOH solubility of 10 wt% and ZnO solubility of 1.0 wt%, the solution is kept for 10s, then concentrated nitric acid with concentration of 50 wt% is used for treating for 30s, a zinc layer on the surface of the substrate is removed, the substrate is immersed into the zinc immersion solution for 10s, and finally, chemical plating is carried out under certain conditions (pH 4.880 ℃/O.5h) to obtain a smooth NiP coating.
Example 1 Cu for aluminum substrate2+/H+After treatment, soaking zinc to obtain a NiP coating; comparative example 1 is a method in which zinc is directly applied to an aluminum substrate to obtain a NiP coating; comparative example 2 is a NiP coating obtained by removing an oxide layer from an aluminum substrate and then soaking in zinc.
Scanning the example 1 and the comparative examples 1-2 by using a scanning electron microscope respectively to obtain an enlarged morphology image of the surface of the aluminum substrate, wherein the morphology image comprises a zinc layer and a NiP coating, as shown in FIG. 2, the roughness of the NiP coating prepared in the example 1 is only 1/4 of the roughness of the NiP coating corresponding to the comparative example 1, and the root-mean-square roughness of the NiP coating is only 5.5 nm. In addition, the concentration was also adjusted to 3.5 wt% NaCl solution and 0.5mol/L H2SO4The solution was tested for corrosion resistance and as shown in fig. 3, the results of the impedance fit analysis showed: through Cu2+/H+The NiP coating after treatment was the most dense. Thus, via Cu2+/H+And (2) treating, namely obtaining a NiP coating with a smoother surface and lower porosity by improving the uniformity of the size and distribution of zinc particles, so that the corrosion resistance of the NiP coating is improved, and the possible principle is as follows: cu2+/H+The thin copper layer after solution treatment can be used as an active point of Zn, which is beneficial to obtaining a smoother Zn layer, and further influences the growth of Ni in the laminated direction, so that the surface smoothness of the NiP coating is greatly improved, and the growth schematic diagrams of the NiP coatings of the embodiment 1 and the comparative example 1 are shown in FIG. 4.
Example 2
The pretreatment method for improving the flatness of the electroless NiP plating layer on the aluminum substrate in the embodiment 2 of the invention comprises the following steps:
(1) selecting pure aluminum foil with the thickness of 200 microns as an aluminum substrate, and performing oil removal treatment on the aluminum substrate, wherein the oil removal current is 4ASD (A/dm)2) The time is about 10s, and the temperature is controlled at 50 ℃; washing with deionized water, and washing with 10 wt% hydrochloric acid solution for 30 s;
(2) immersing an aluminum substrate in Cu2+Concentration of 2 × 10-3mol/L，H+Treating the mixture for 40s at 70 ℃ in a solution with the concentration of 10 mol/L;
(3) at room temperature, an aluminum substrate is immersed into a zinc immersion solution with NaOH solubility of 10 wt% and ZnO solubility of 1.0 wt%, the solution is kept for 10s, then concentrated nitric acid with concentration of 50 wt% is used for treating for 30s, a zinc layer on the surface of the substrate is removed, the substrate is immersed into the zinc immersion solution again for 10s, and finally, chemical plating is carried out under certain conditions (pH 4.880 ℃/0.5h) to obtain a flat NiP plating layer.
Example 3
The pretreatment method for improving the flatness of the electroless NiP plating layer on the aluminum substrate in the embodiment 3 of the invention comprises the following steps:
(1) selecting pure aluminum foil with the thickness of 200 microns as an aluminum substrate, and performing oil removal treatment on the aluminum substrate, wherein the oil removal current is 4ASD (A/dm)2) The time is about 10s, and the temperature is controlled at 50 ℃; washing with deionized water, and washing with 10 wt% hydrochloric acid solution for 30 s;
(2) immersing an aluminum substrate in Cu2+The concentration is 0.5 × 10-3mol/L，H+Treating the mixture for 50s at 70 ℃ in a solution with the concentration of 10 mol/L;
(3) at room temperature, an aluminum substrate is immersed into a zinc immersion solution with NaOH solubility of 10 wt% and ZnO solubility of 1.0 wt%, the solution is kept for 10s, then concentrated nitric acid with concentration of 50 wt% is used for treating for 30s, a zinc layer on the surface of the substrate is removed, the substrate is immersed into the zinc immersion solution again for 10s, and finally, chemical plating is carried out under certain conditions (pH 4.880 ℃/0.5h) to obtain a flat NiP plating layer.
Example 4
The pretreatment method for improving the flatness of the electroless NiP plating layer on the aluminum substrate in the embodiment 4 of the invention comprises the following steps:
(1) selecting pure aluminum foil with the thickness of 200 microns as an aluminum substrate, and performing oil removal treatment on the aluminum substrate, wherein the oil removal current is 4ASD (A/dm)2) The time is about 10s, and the temperature is controlled at 50 ℃; washing with deionized water, and washing with 10 wt% hydrochloric acid solution for 30 s;
(2) immersing an aluminum substrate in Cu2+The concentration is 2.0 × 10-3mol/L，H+Treating the mixture for 40s at 20 ℃ in a solution with the concentration of 15 mol/L;
(3) at room temperature, an aluminum substrate is immersed into a zinc immersion solution with NaOH solubility of 10 wt% and ZnO solubility of 1.0 wt%, the solution is kept for 10s, then concentrated nitric acid with concentration of 50 wt% is used for treating for 30s, a zinc layer on the surface of the substrate is removed, the substrate is immersed into the zinc immersion solution again for 10s, and finally, chemical plating is carried out under certain conditions (pH 4.880 ℃/0.5h) to obtain a flat NiP plating layer.
Example 5
The pretreatment method for improving the flatness of the electroless NiP plating layer on the aluminum substrate in the embodiment 5 of the invention comprises the following steps:
(1) selecting pure aluminum foil with the thickness of 200 microns as an aluminum substrate, and performing oil removal treatment on the aluminum substrate, wherein the oil removal current is 4ASD (A/dm)2) The time is about 10s, and the temperature is controlled at 50 ℃; washing with deionized water, and washing with 10 wt% hydrochloric acid solution for 30 s;
(2) immersing an aluminum substrate in Cu2+The concentration is 2.0 × 10-3mol/L，H+Treating the mixture for 40s at 80 ℃ in a solution with the concentration of 5 mol/L;
(3) at room temperature, an aluminum substrate is immersed into a zinc immersion solution with NaOH solubility of 10 wt% and ZnO solubility of 1.0 wt%, the solution is kept for 10s, then concentrated nitric acid with concentration of 50 wt% is used for treating for 30s, a zinc layer on the surface of the substrate is removed, the substrate is immersed into the zinc immersion solution again for 10s, and finally, chemical plating is carried out under certain conditions (pH 4.880 ℃/0.5h) to obtain a flat NiP plating layer.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims (7)

1. A pretreatment method for improving the flatness of an electroless NiP plating layer of an aluminum substrate is characterized by comprising the following steps:
(1) selecting an aluminum substrate material, and carrying out oil removal and acid pickling pretreatment on the aluminum substrate material to clean the surface of the aluminum substrate material;
(2) then dipping it into Cu2+In an acidic solution to deposit copper on the surface thereof, wherein the Cu is contained2+In an acidic solution of Cu2+Has a solubility of 0.5 × 10-3～2×10-3mol/L，H+In a concentration of 5.0 ℃15.0mol/L, the temperature is 20-80 ℃, and the time is 30-50 s;
(3) soaking the substrate in a zinc soaking solution for secondary zinc soaking, wherein the zinc soaking solution is a mixed solution of NaOH and ZnO; and finally, carrying out chemical plating to obtain a NiP plating layer on the aluminum substrate.
2. The pretreatment method for improving the flatness of an electroless NiP plating layer on an aluminum substrate according to claim 1, wherein said aluminum substrate is made of pure aluminum or an aluminum alloy.
3. The pretreatment method for improving the flatness of an electroless NiP plating layer on an aluminum substrate according to claim 1, wherein the pickling solution contains hydrochloric acid having a solubility of 5 to 15 wt%.
4. The pretreatment method for improving the flatness of an electroless NiP plating layer on an aluminum substrate according to claim 1, wherein in the step (3), the zinc dipping solution has a NaOH concentration of 5-20 wt% and a ZnO concentration of 0.1-5.0 wt%.
5. The pretreatment method for improving the flatness of the electroless NiP plating layer on the aluminum substrate according to claim 4, wherein in the step (3), the zincating temperature is 20-30 ℃ and the zincating time is 10-60 s.
6. The pretreatment method for improving the flatness of an electroless NiP plating layer on an aluminum substrate according to claim 1, wherein in the step (3), the dezincification solution is HNO3The concentration of the solution is 20-60 wt%.
7. The pretreatment method for improving the flatness of an electroless NiP plating layer on an aluminum substrate according to claim 6, wherein in the step (3), the temperature for removing zinc is 20-30 ℃ and the time for removing zinc is 5-30 s.
CN202010267177.3A 2020-04-07 2020-04-07 Pretreatment method for improving flatness of electroless NiP plating layer on aluminum substrate Pending CN111364030A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
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CN114134491A (en) * 2021-12-03 2022-03-04 广东工业大学 Method for improving internal roughness of aluminum-based copper-clad plate hole
WO2024060342A1 (en) * 2022-09-22 2024-03-28 江苏富乐华半导体科技股份有限公司 Method for improving thermal cycle reliability of aluminum nitride direct-bonded aluminum packaging substrate

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