CN111155075A - Secondary metallization method for special-shaped ceramic - Google Patents
Secondary metallization method for special-shaped ceramic Download PDFInfo
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- CN111155075A CN111155075A CN201911413250.7A CN201911413250A CN111155075A CN 111155075 A CN111155075 A CN 111155075A CN 201911413250 A CN201911413250 A CN 201911413250A CN 111155075 A CN111155075 A CN 111155075A
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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
- C23C18/42—Coating with noble metals
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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
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
- C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
-
- 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
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1875—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment only one step pretreatment
- C23C18/1882—Use of organic or inorganic compounds other than metals, e.g. activation, sensitisation with polymers
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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
Abstract
The invention provides a secondary metallization method for special-shaped ceramic, which comprises the following steps: and (3) sequentially carrying out ultrasonic cleaning, acid activation, palladium precipitation, hanging replacement, nickel presoaking and chemical nickel plating on the special-shaped ceramic subjected to molybdenum-manganese sintering treatment, and cleaning to obtain the special-shaped ceramic with secondarily metallized surface. According to the invention, through controlling various process parameters in the palladium deposition and nickel plating processes in a cooperative control manner, the nickel can be coated on the molybdenum-manganese layer of the special-shaped ceramic, and the surface of the ceramic which is not coated with the molybdenum-manganese layer is not coated with nickel.
Description
Technical Field
The invention belongs to the technical field of electroplating, and particularly relates to a secondary metallization method for special-shaped ceramic.
Background
Currently, electroplating is generally used to perform local secondary metallization on each surface of the ceramic shell, and these electroplating methods generally include: roll plating, forcing nickel in chemical nickel, rack plating, rack plating chemical nickel, roll chemical plating, and the like. Because the shapes of the shells of the special-shaped ceramics are different, a plurality of small holes are usually formed in the surfaces of the shells, matched hangers cannot be manufactured easily in the electroplating process, chemical nickel is usually adopted to force nickel to be added, or copper wires are bound to carry out barrel plating, but the methods are only limited to small-batch production and cannot realize large-scale production. The special-shaped ceramic used as the relay shell has high requirement on air tightness, a metal coating generated by barrel plating is easy to damage, and a copper wire is bound, so that manual operation is required, time and labor are wasted, and scratches are easily generated on a nickel layer. When nickel is sequentially forced on a plurality of parts of the special-shaped ceramic, the thickness of each part nickel layer is inconsistent due to time difference, and the service performance of the special-shaped ceramic after metallization is influenced.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects and shortcomings in the background technology and providing a secondary metallization method for special-shaped ceramics.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a secondary metallization method for special-shaped ceramics comprises the following steps:
and (3) sequentially carrying out ultrasonic cleaning, acid activation, palladium precipitation, hanging replacement, nickel presoaking and chemical nickel plating on the special-shaped ceramic subjected to molybdenum-manganese sintering treatment, and cleaning to obtain the special-shaped ceramic with secondarily metallized surface.
In the secondary metallization method of the special-shaped ceramic, the palladium deposition temperature is preferably 20-30 ℃, and the palladium deposition time is preferably 2-3 minutes.
In the method for secondarily metallizing the special-shaped ceramic, the palladium precipitation solution preferably contains palladium ions with the concentration of 40-60ppm and sulfuric acid with the concentration of 1-2 mol/L. The palladium salt providing palladium ions in the palladium precipitation solution is palladium sulfate, and anions such as chloride ions in the rest of the palladium salts influence the penetration of nickel to the ceramic, so that the overflow plating occurs.
The secondary metallization method of the special-shaped ceramic is preferred, soThe nickel plating solution of the pre-dipped nickel plating contains NaH with the concentration of 50-120g/L2PO2.·H2O and 150g/L NaOH with the concentration of 100-.
In the secondary metallization method for the special-shaped ceramic, the temperature of the pre-immersion nickel plating is preferably 40-60 ℃ and the time is preferably 1-2 minutes.
In the above-mentioned secondary metallization method for the special-shaped ceramic, preferably, the nickel plating solution of the electroless nickel plating contains MK689A with a concentration of 90-110ml/L, MK689B with a concentration of 90-110ml/L and MK689C with a concentration of 180-240 ml/L. The main component of MK689A in the invention is nickel sulfate, the concentration of nickel ions is 3-6g/L, and the manufacturer is Guangzhou McGinko electronic materials Co; the main component of MK689B is sodium hypophosphite with a concentration of 10-15g/L, and the manufacturer is McGinko electronic materials, Guangzhou; the MK689C mainly comprises complexing agent including two or three of sodium citrate, malic acid and succinic acid, the total content of the complexing agent is 30-60g/L, and the manufacturer is Guangzhou McGico electronic materials Co.
In the secondary metallization method of the special-shaped ceramic, the temperature of the chemical nickel plating is preferably 40-50 ℃ and the time is preferably 40-60 minutes.
Preferably, the ultrasonic cleaning is carried out in a detergent at the temperature of 50-60 ℃ for 2-5 minutes, and then the special-shaped ceramic is cleaned by deionized water after the ultrasonic cleaning. The detergent is usually selected from a detergent which contains surfactants such as nonylphenol polyoxyethylene ether and the like, and the content of the surfactants is 5-10 ml/l.
In the method for secondarily metallizing the special-shaped ceramic, preferably, the acid activation is carried out in a sulfuric acid solution, the concentration of the sulfuric acid is 1-2mol/L, the temperature of the acid activation is 20-30 ℃, and the time is 30-60 seconds.
Compared with the prior art, the invention has the advantages that:
according to the secondary metallization method for the special-shaped ceramic, various process parameters in the palladium deposition and nickel plating processes are controlled in a coordinated mode, the molybdenum-manganese layer of the special-shaped ceramic can be plated with nickel, the surface of the ceramic which is not coated with the molybdenum-manganese layer is not plated with nickel, the process is stable, the operation is simple, the production efficiency is high, and the secondary metallization method is suitable for mass production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a photograph of a shaped ceramic obtained after secondary metallization in example 1 of the present invention;
FIG. 2 is a photograph of a shaped ceramic obtained after secondary metallization in example 2 of the present invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the invention relates to a secondary metallization method of special-shaped ceramic, which comprises the following steps:
(1) carrying out ultrasonic cleaning and acid activation on the special-shaped ceramic with the porous structure after molybdenum-manganese sintering treatment, wherein the ultrasonic cleaning is carried out in a Libai detergent with the concentration of 5ml/l, the ultrasonic cleaning temperature is 55 ℃, the ultrasonic cleaning time is 5 minutes, and the special-shaped ceramic is cleaned by deionized water after the ultrasonic cleaning; the acid activation is carried out in a sulfuric acid solution, the concentration of the sulfuric acid is 1mol/L, the temperature of the acid activation is 25 ℃, and the time is 30 seconds;
(2) performing palladium precipitation on the special-shaped ceramic obtained in the step (1), wherein the palladium precipitation temperature is 25 ℃, the palladium precipitation time is 1 minute, and palladium ions with the concentration of 50ppm and sulfuric acid with the concentration of 1mol/L are contained in a palladium precipitation solution;
(3) after replacement and hanging, the special-shaped ceramics obtained in the step (2) are pre-dipped with nickel, and the nickel plating solution contains NaH with the concentration of 120g/L2PO2.·H2O and NaOH with the concentration of 100g/L, wherein the temperature of the nickel pre-dip plating is 55 ℃, and the time is 1 minute;
(4) performing chemical nickel plating on the special-shaped ceramic obtained in the step (3), wherein the nickel plating solution contains MK689A with the concentration of 100ml/L, MK689B with the concentration of 100ml/L and MK689C with the concentration of 200ml/L, and all manufacturers of MK689A, MK689B and MK689C are Kyoco electronic materials, Guangzhou, the temperature of the chemical nickel plating is controlled to be 48 ℃, and the time is 45 minutes; after the chemical nickel plating is finished, cleaning to obtain the special-shaped ceramic with the secondarily metallized surface, wherein a photo of a product is shown in figure 1, and it can be seen that the molybdenum-manganese layer of the special-shaped ceramic can be coated with nickel, the surface of the ceramic which is not coated with the molybdenum-manganese layer is not coated with nickel, and the thickness of the nickel layer is 2.5-4.0 um. The method has the advantages of stable process, simple operation, good nickel effect on the molybdenum-manganese layer and mass production.
Example 2:
the invention relates to a secondary metallization method of special-shaped ceramic, which comprises the following steps:
(1) carrying out ultrasonic cleaning and acid activation on the special-shaped ceramic with the porous structure after molybdenum-manganese sintering treatment, wherein the ultrasonic cleaning is carried out in a Libai detergent with the concentration of 10ml/l, the ultrasonic cleaning temperature is 50 ℃, the ultrasonic cleaning time is 2 minutes, and the special-shaped ceramic is cleaned by deionized water after the ultrasonic cleaning; the acid activation is carried out in a sulfuric acid solution, the concentration of the sulfuric acid is 2mol/L, the temperature of the acid activation is 30 ℃, and the time is 50 seconds;
(2) performing palladium precipitation on the special-shaped ceramic obtained in the step (1), wherein the palladium precipitation temperature is 25 ℃, the palladium precipitation time is 2 minutes, and palladium ions with the concentration of 40ppm and sulfuric acid with the concentration of 2mol/L are contained in a palladium precipitation solution;
(3) after replacing and hanging, the special-shaped ceramics obtained in the step (2) are pre-dipped with nickel, and the nickel plating solution containsWith NaH at a concentration of 100g/L2PO2.·H2O and NaOH with the concentration of 150g/L, wherein the temperature of the nickel presoaking is 50 ℃, and the time is 2 minutes;
(4) performing chemical nickel plating on the special-shaped ceramic obtained in the step (3), wherein the nickel plating solution contains MK689A with the concentration of 90ml/L, MK689B with the concentration of 110ml/L and MK689C with the concentration of 220ml/L, and all manufacturers of MK689A, MK689B and MK689C are Kyoco electronic materials, Inc. in Guangzhou, the temperature of the chemical nickel plating is controlled to be 45 ℃ and the time is 42 minutes; after the chemical nickel plating is finished, cleaning to obtain the special-shaped ceramic with the secondarily metallized surface, wherein a photo of a product is shown in figure 2, and it can be seen that the molybdenum-manganese layer of the special-shaped ceramic can be coated with nickel, while the surface of the ceramic which is not coated with the molybdenum-manganese layer is not coated with nickel, and the thickness of the nickel layer is 2.0-4.5 um. The method has the advantages of stable process, simple operation, good nickel effect on the molybdenum-manganese layer and mass production.
Claims (9)
1. A secondary metallization method for special-shaped ceramics is characterized by comprising the following steps:
and (3) sequentially carrying out ultrasonic cleaning, acid activation, palladium precipitation, hanging replacement, nickel presoaking and chemical nickel plating on the special-shaped ceramic subjected to molybdenum-manganese sintering treatment, and cleaning to obtain the special-shaped ceramic with secondarily metallized surface.
2. The secondary metallization method of a shaped ceramic according to claim 1, wherein the palladium deposition temperature is 20-30 ℃ and the palladium deposition time is 2-3 minutes.
3. The secondary metallization method of the special-shaped ceramic as claimed in claim 1, wherein the palladium precipitation solution contains palladium ions with a concentration of 40-60ppm and sulfuric acid with a concentration of 1-2 mol/L.
4. The secondary metallization method of shaped ceramics according to claim 1, wherein the plating solution of pre-impregnated nickel contains NaH with concentration of 50-120g/L2PO2.·H2O and 150g/L NaOH with the concentration of 100-.
5. The secondary metallization method of a shaped ceramic according to claim 1, wherein the pre-impregnated nickel is at a temperature of 40-60 ℃ for 1-2 minutes.
6. The secondary metallization method of special-shaped ceramic as claimed in claim 1, wherein the electroless nickel plating solution contains MK689A with a concentration of 90-110ml/L, MK689B with a concentration of 90-110ml/L and MK689C with a concentration of 180-240 ml/L.
7. The secondary metallization method of a shaped ceramic according to claim 1, wherein the electroless nickel plating is performed at a temperature of 40-50 ℃ for a time of 40-60 minutes.
8. The secondary metallization method of the special-shaped ceramic according to claim 1, wherein the ultrasonic cleaning is performed in a detergent, the temperature of the ultrasonic cleaning is 50-60 ℃, the time is 2-5 minutes, and the ultrasonic cleaning is performed and then the cleaning is performed by using deionized water.
9. The secondary metallization method of shaped ceramics according to claim 1, characterized in that the acid activation is carried out in sulfuric acid solution, the concentration of sulfuric acid is 1-2mol/L, the temperature of acid activation is 20-30 ℃, and the time is 30-60 seconds.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114540801A (en) * | 2020-11-24 | 2022-05-27 | 娄底市安地亚斯电子陶瓷有限公司 | Nickel plating process suitable for ceramic sealing connector |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114540801A (en) * | 2020-11-24 | 2022-05-27 | 娄底市安地亚斯电子陶瓷有限公司 | Nickel plating process suitable for ceramic sealing connector |
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Application publication date: 20200515 |