CN111778498B - Coating structure and preparation method thereof - Google Patents

Coating structure and preparation method thereof Download PDF

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Publication number
CN111778498B
CN111778498B CN202010634498.2A CN202010634498A CN111778498B CN 111778498 B CN111778498 B CN 111778498B CN 202010634498 A CN202010634498 A CN 202010634498A CN 111778498 B CN111778498 B CN 111778498B
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layer
silver
acid
palladium
chemical
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CN111778498A (en
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刘彬灿
黄明起
夏建文
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Shenzhen Samcien Semiconductor Materials Co ltd
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Shenzhen Samcien Semiconductor Materials Co ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/16Chemical 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
    • C23C18/31Coating with metals
    • C23C18/42Coating with noble metals
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/16Chemical 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
    • C23C18/31Coating with metals
    • C23C18/42Coating with noble metals
    • C23C18/44Coating with noble metals using reducing agents
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/54Contact plating, i.e. electroless electrochemical plating
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C28/00Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/02Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
    • C23C28/023Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only

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

Abstract

The invention discloses a coating structure and a preparation method thereof. The coating structure comprises a silver layer, a palladium layer and a gold layer which are sequentially arranged on the conductive layer. Aiming at the problems that the prior art of nickel-palladium-gold is that a layer of palladium is deposited on a nickel layer in a deposition mode and then a layer of gold is deposited in a displacement mode, loss and attenuation are caused during high-frequency and high-speed signal transmission due to the magnetism of the nickel layer, and the high-frequency and high-speed signal transmission cannot be met. The coating structure provided by the invention comprises a silver layer, a palladium layer and a gold layer, has no magnetism, does not influence signal high-frequency and high-speed transmission, can protect a conductive layer and provides good weldability, conductivity, corrosion resistance, friction resistance and the like. The silver layer replaces gold (noble metal) and the cost is obviously reduced, the palladium layer on the surface of the silver can effectively prevent the silver layer from being corroded, and the gold layer can play roles of wetting and corrosion resistance.

Description

Coating structure and preparation method thereof
Technical Field
The invention belongs to the technical field of surface treatment, and particularly relates to a coating structure and a preparation method thereof.
Background
In the existing packaging technology of electronic industrial parts, nickel-palladium-gold is widely applied to industry as a traditional surface treatment mode, and the surface of a conducting layer is provided with the characteristics of excellent gold wire bonding performance, wear resistance, corrosion resistance and the like.
With the development of science, people walk into the 5G era, meanwhile, electronic industrial component packages such as semiconductor packages, IC substrates, aluminum substrates, ceramic substrates, printed circuit boards and the like are marked to enter a high-frequency and high-speed period, nickel palladium gold is used as a traditional surface treatment process, and the existing surface treatment materials limit the development of high frequency and high speed because of the loss and attenuation caused by the magnetism of a nickel layer and the signal during high-frequency and high-speed transmission.
The Jin Bajin coating has excellent bonding and welding performance equal to those of a nickel-palladium-gold coating, but has the defects of higher processing cost and difficult maintenance of mass production because three layers of the laminated structure are all composed of noble metals.
CN102605359a discloses a novel surface treatment stack of electroless palladium-gold plating film, on the bonding pad (copper), firstly forming a layer of 0.06-0.12 μm metal palladium by using a displacement type method, then depositing a layer of 0.03-0.2 μm reduced palladium layer on the displacement type palladium layer for thickening the palladium plating layer, finally depositing a layer of 0.03-0.2 μm gold on the palladium surface by using a reduction method. Because gold is deposited in an oxidation-reduction mode, the stability of bath solution is poor, management and control are difficult in the actual production and processing process, the requirement of large-scale mass production is difficult to meet, the palladium layer is used as a copper ion shielding layer, the thickness of the palladium layer is required to be thicker, the cost of palladium used as a noble metal is higher, and the application of the palladium in the industrial production end is more limited.
CN110241406a and CN110318047a disclose another surface treatment stack of electroless gold palladium gold plating film, wherein a layer of thin gold is replaced on a bonding pad (copper) by using a replacement mode, then a layer of electroless palladium is deposited on a gold surface by using the catalytic property of gold, and finally a layer of electroless gold is deposited on palladium by using a replacement mode, so that the chemical stack of Jin Bajin is finally formed, and because three layers of the stack structure are all composed of noble metals, the processing cost is high, and mass production is difficult to maintain.
Therefore, there is a need in the art to develop a novel plating film preparation method which has the advantages of better solderability, conductivity and corrosion resistance, no loss and attenuation of signals during high-frequency and high-speed transmission, and lower production cost.
Disclosure of Invention
Aiming at the problems that the prior art nickel-palladium-gold is formed by depositing a layer of palladium on a nickel layer in a deposition mode and then depositing a layer of gold in a displacement mode, the loss and attenuation can be caused during high-frequency and high-speed signal transmission due to the magnetism of the nickel layer, and the high-frequency and high-speed signal transmission cannot be met, the invention aims to provide a film coating structure and a preparation method thereof. The coating film obtained by the method has the advantages of no magnetism, no influence on high-frequency and high-speed signal transmission, good weldability, conductivity, wear resistance and the like.
In order to achieve the above purpose, the invention adopts the following technical scheme:
One of the purposes of the present invention is to provide a plating structure, which comprises a silver layer, a palladium layer and a gold layer sequentially arranged on a conductive layer.
The coating structure comprises a silver layer, a palladium layer and a gold layer, has no magnetism, does not influence high-frequency and high-speed signal transmission, can protect a conductive layer and provides good weldability, conductivity, corrosion resistance, friction resistance and the like. The silver layer replaces gold (noble metal) and the cost is obviously reduced, the palladium layer on the surface of the silver can effectively prevent the silver layer from being corroded, and the gold layer can play roles of wetting and corrosion resistance.
Preferably, the silver layer has a thickness of 0.2 to 0.4 μm, for example 0.21 μm, 0.23 μm, 0.25 μm, 0.27 μm, 0.29 μm, 0.3 μm, 0.31 μm, 0.33 μm, 0.35 μm, 0.37 μm or 0.39 μm, etc.
Preferably, the palladium layer has a thickness of 0.05 to 0.2 μm, for example 0.06 μm, 0.07 μm, 0.08 μm, 0.09 μm, 0.1 μm, 0.11 μm, 0.12 μm, 0.13 μm, 0.14 μm, 0.15 μm, 0.16 μm, 0.17 μm, 0.18 μm or 0.19 μm, etc.
Preferably, the gold layer has a thickness of 0.05 to 0.2 μm, for example 0.06 μm, 0.07 μm, 0.08 μm, 0.09 μm, 0.1 μm, 0.11 μm, 0.12 μm, 0.13 μm, 0.14 μm, 0.15 μm, 0.16 μm, 0.17 μm, 0.18 μm or 0.19 μm, etc.
Another object of the present invention is to provide a method for manufacturing a plating film structure as defined in one of the objects, the method comprising: and sequentially preparing a silver layer, a palladium layer and a gold layer on the conductive layer to obtain a coating structure.
According to the invention, a layer of chemical silver is firstly replaced on the conductive layer in a replacement mode, then a layer of metal palladium is deposited in a redox mode through self-catalysis of silver, so that corrosion of the silver layer can be effectively prevented, and finally a layer of gold is deposited in a redox mode to play a role in wetting and corrosion resistance.
Compared with Jin Bajin film coating structure, the invention uses silver to replace gold (noble metal), the cost is obviously reduced and the cost is also obviously reduced; compared with a nickel-palladium-gold coating structure, the invention has the advantages of simpler coating process, lower operating temperature and indirectly reduced cost.
Preferably, the preparation method of the silver layer comprises the following steps: and carrying out displacement reaction on the conductive layer to obtain the silver layer.
Preferably, the preparation method of the silver layer comprises the following steps: and placing the conductive layer in a chemical silver solution to obtain the conductive layer with the surface covered with the silver layer.
Preferably, the pH of the chemical silver solution is 8.0 to 9.0, such as 8.1, 8.2, 8.3, 8.4, 8.5, 8.6, 8.7, 8.8 or 8.9, etc.
Preferably, the temperature of the chemical silver solution is 40 to 70 ℃, for example, 42 ℃, 45 ℃, 48 ℃, 50 ℃, 52 ℃, 55 ℃, 58 ℃, 60 ℃, 62 ℃, 65 ℃, 68 ℃, or the like.
Preferably, the conductive layer is placed in the chemical silver solution for a period of time ranging from 2 to 4 minutes, such as 2.5 minutes, 3 minutes, or 3.5 minutes, etc.
Preferably, after the silver layer is prepared on the conductive layer, a washing process is further included, preferably washing with pure water.
Preferably, the chemical silver solution comprises silver ions or complex silver ions, preferably the chemical silver solution further comprises any one or a combination of at least two of an amine complexing agent, an amino complexing agent and a polyhydroxy acid complexing agent, and further preferably the chemical silver solution consists of silver ions or complex silver ions, an amine complexing agent, an amino complexing agent and a polyhydroxy acid complexing agent.
Preferably, the concentration of silver ions or complex silver ions in the chemical silver solution is 0.5 to 5g/L, for example 1g/L, 1.5g/L, 2g/L, 2.5g/L, 3g/L, 3.5g/L, 4g/L or 4.5g/L, etc.
Preferably, in the chemical silver solution, the concentration of the amine complexing agent is 1-20 g/L, such as 3g/L, 5g/L, 7g/L, 9g/L, 10g/L, 11g/L, 13g/L, 15g/L, 17g/L or 19g/L, etc.
Preferably, in the chemical silver solution, the concentration of the amino complexing agent is 1-20 g/L, such as 3g/L, 5g/L, 7g/L, 9g/L, 10g/L, 11g/L, 13g/L, 15g/L, 17g/L, 19g/L, etc.
Preferably, the concentration of the polyhydroxy acid complexing agent in the chemical silver solution is 1 to 20g/L, such as 3g/L, 5g/L, 7g/L, 9g/L, 10g/L, 11g/L, 13g/L, 15g/L, 17g/L, 19g/L, etc.
Preferably, the silver ion or the complex silver ion includes any one or a combination of at least two of a silver ammonia complex ion, a silver sulfite complex ion and a silver halide complex ion.
Preferably, the amine complexing agent comprises any one or a combination of at least two of ammonia water, triamine citrate, ammonium phosphate, ammonium sulfate, ammonium nitrate, ammonium acetate, ammonium ethylene diamine carbonate, diethylenetriamine, aminopyridine of triethylenetetramine, aniline and phenylenediamine.
Preferably, the amino complexing agent comprises any one or a combination of at least two of glycine, alpha-alanine, beta-alanine, cystine, ethylenediamine tetraacetic acid, aspartic acid, glutamic acid, sulfamic acid nitrilotriacetic acid and aromatic cyclic amino acids.
Preferably, the polyhydroxy acid complexing agent comprises any one or a combination of at least two of an acid, an alkali metal salt of the acid and an ammonium salt of the acid, preferably any one or a combination of at least two of citric acid, tartaric acid, gluconic acid, malic acid, lactic acid, 1-hydroxy-ethylidene-1, 1-diphosphate, sulfosalicylic acid and phthalic acid.
Preferably, the preparation method of the palladium layer comprises the following steps: and depositing a layer of metal palladium on the silver layer in a redox mode to obtain a palladium layer.
Preferably, the preparation method of the palladium layer comprises the following steps: and placing the conductive layer with the surface covered with the silver layer in a chemical palladium solution to obtain a pre-product, wherein the palladium layer in the pre-product is covered on the surface of the silver layer.
Preferably, the pH of the electroless palladium solution is 6.5 to 8.0, such as 6.6, 6.7, 6.8, 6.9, 7.0, 7.1, 7.2, 7.3, 7.4, 7.5, 7.6, 7.7, 7.8, or 7.9, etc.
Preferably, the temperature of the chemical palladium solution is 40 to 70 ℃, for example, 42 ℃, 45 ℃, 48 ℃, 50 ℃, 52 ℃, 55 ℃, 58 ℃, 60 ℃, 62 ℃, 65 ℃, 68 ℃, or the like.
Preferably, the conductive layer with the silver layer covered on the surface is placed in the chemical palladium solution for 4-15 min, for example, 5min, 6min, 8min, 10min, 12min or 14min, etc.
Preferably, after the pre-product is obtained, a washing process is also included, preferably with pure water.
Preferably, the chemical palladium solution comprises palladium salt, preferably the chemical palladium solution further comprises any one or a combination of at least two of a main complexing agent, an auxiliary complexing agent, a reducing agent, a first stabilizer and a first pH buffer, further preferably the chemical palladium solution consists of palladium ions or palladium complex ions, a main complexing agent, an auxiliary complexing agent, a reducing agent, a first stabilizer and a first pH buffer.
Preferably, the palladium salt concentration is 0.1 to 5g/L, for example 0.2g/L, 0.5g/L, 0.8g/L, 1g/L, 1.5g/L, 2g/L, 2.5g/L, 3g/L, 3.5g/L, 4g/L, 4.5g/L, etc.
Preferably, the concentration of the primary complexing agent is 5 to 20g/L, such as 6g/L, 7g/L, 9g/L, 10g/L, 11g/L, 13g/L, 15g/L, 17g/L, 19g/L, etc.
Preferably, the concentration of the auxiliary complexing agent is 5-25 g/L, for example 6g/L, 7g/L, 9g/L, 10g/L, 11g/L, 13g/L, 15g/L, 17g/L, 19g/L, 20g/L, 22g/L, 23g/L, 24g/L, etc.
Preferably, the concentration of the reducing agent is 1 to 25g/L, for example 3g/L, 5g/L, 8g/L, 10g/L, 11g/L, 13g/L, 15g/L, 17g/L, 19g/L, 20g/L, 22g/L, 23g/L, 24g/L, etc.
Preferably, the concentration of the first stabilizer is 0.1 to 5mg/L, for example 0.2mg/L, 0.5mg/L, 0.8mg/L, 1mg/L, 1.5mg/L, 2mg/L, 2.5mg/L, 3mg/L, 3.5mg/L, 4mg/L, 4.5mg/L, etc.
Preferably, the concentration of the first pH buffer is 0.5 to 5g/L, for example 0.8g/L, 1g/L, 1.5g/L, 2g/L, 2.5g/L, 3g/L, 3.5g/L, 4g/L, 4.5g/L, etc.
Preferably, the palladium salt includes any one or a combination of at least two of palladium sulfate, palladium chloride, ammonium palladium chloride, tetra-ammine palladium dichloride and ammine palladium sulfate.
Preferably, the main complexing agent is an amine-based compound, preferably comprising any one or a combination of at least two of ammonia, ethylenediamine, ethylamine and sodium ethylenediamine tetraacetate.
Preferably, the auxiliary complexing agent comprises any one or a combination of at least two of sodium citrate, acrylic acid, succinic acid, oxalic acid and malic acid.
Preferably, the reducing agent comprises any one or a combination of at least two of formic acid, hypophosphite, ascorbic acid and dimethylamine borane.
Preferably, the first stabilizer comprises any one or a combination of at least two of bismuth nitrate, thiourea, 4-dimethylaminopyridine and 2-mercaptobenzothiophene.
Preferably, the first pH buffer comprises any one or a combination of at least two of borax, boric acid, sodium dihydrogen phosphate and disodium hydrogen phosphate.
Preferably, the preparation method of the gold layer comprises the following steps: and depositing a layer of gold on the surface of the pre-product in a redox mode to obtain a gold layer.
Preferably, the preparation method of the gold layer comprises the following steps: and placing the pre-product in a chemical gold solution to obtain a coating structure.
Preferably, the pH of the electroless gold solution is between 6.0 and 7.0, such as 6.1, 6.2, 6.3, 6.4, 6.5, 6.6, 6.7, 6.8 or 6.9, etc.
Preferably, the temperature of the electroless gold solution is 70 to 80 ℃, for example, 71 ℃, 72 ℃, 73 ℃, 74 ℃, 75 ℃, 76 ℃, 77 ℃, 78 ℃, 79 ℃, or the like.
Preferably, the pre-product is placed in the electroless gold solution for a period of time ranging from 0.5 to 20 minutes, such as 0.6, 1, 5, 8, 10, 12, 15, 18, 19, etc.
Preferably, after the film-plating structure is obtained, a washing and drying process is further included, preferably washing with pure water.
Preferably, the temperature of the drying is 60 to 90 ℃, for example 62 ℃, 65 ℃, 68 ℃, 70 ℃, 72 ℃, 75 ℃, 78 ℃, 80 ℃, 82 ℃, 85 ℃, 88 ℃, or the like.
Preferably, the chemical gold solution comprises a gold salt, preferably the chemical gold solution further comprises any one or a combination of at least two of a complexing agent, an accelerator, a second stabilizer and a second pH buffer, further preferably the chemical gold solution consists of a gold salt, a complexing agent, an accelerator, a second stabilizer and a second pH buffer.
Preferably, the concentration of gold salt in the electroless gold solution is 0.1 to 5g/L, for example 0.2g/L, 0.5g/L, 0.8g/L, 1g/L, 1.5g/L, 2g/L, 2.5g/L, 3g/L, 3.5g/L, 4g/L, 4.5g/L, etc.
Preferably, the concentration of complexing agent in the electroless gold solution is 5 to 20g/L, for example 6g/L, 7g/L, 9g/L, 10g/L, 11g/L, 13g/L, 15g/L, 17g/L or 19g/L, etc.
Preferably, the concentration of the accelerator in the electroless gold solution is 1 to 25mg/L, for example, 3mg/L, 5mg/L, 8mg/L, 10mg/L, 11mg/L, 13mg/L, 15mg/L, 17mg/L, 19mg/L, 20mg/L, 22mg/L, 23mg/L, 24mg/L, or the like.
Preferably, the concentration of the second stabilizer in the electroless gold solution is 0.1 to 5mg/L, for example 0.2mg/L, 0.5mg/L, 0.8mg/L, 1mg/L, 1.5mg/L, 2mg/L, 2.5mg/L, 3mg/L, 3.5mg/L, 4mg/L, 4.5mg/L, etc.
Preferably, the concentration of the second pH buffer in the electroless gold solution is 1 to 25g/L, such as 3g/L, 5g/L, 8g/L, 10g/L, 11g/L, 13g/L, 15g/L, 17g/L, 19g/L, 20g/L, 22g/L, 23g/L, 24g/L, etc.
Preferably, the gold salt comprises any one or a combination of at least two of potassium aurous cyanide, potassium aurous citrate, gold chloride and tetrachloric acid hydrate.
Preferably, the complexing agent comprises any one or a combination of at least two of acetohydroxamic acid, benzohydroxamic acid, salicylhydroxamic acid and acetohydroxamic acid.
Preferably, the accelerator comprises any one or a combination of at least two of lanthanum sulfate, cerium sulfate and thallium sulfate.
Preferably, the second stabilizer comprises any one or a combination of at least two of 2, 2-dipyridylamine, 2, 4-dimethylpyridine, 2, 4-dimethylpiperidine, and pyridine-2, 3-dicarboxylic acid.
Preferably, the second pH buffer is any one or a combination of at least two of 2-morpholinoethanesulfonic acid, bis (2-hydroxyethylamino) trimethylol methane, piperazine-1, 4-diethylsulfonic acid, and citric acid-sodium citrate buffer.
Preferably, the conductive layer further comprises a process of degreasing, washing and microetching before the silver layer is prepared.
The invention can improve the conductivity and the mechanical property between the conductive layer and the silver layer by a series of pretreatment (surface cleaning and roughening) on the conductive layer before the silver-palladium-gold is chemically deposited.
The specific composition of the conductive layer is not limited in the present invention, and may be selected by those skilled in the art according to practical situations, and the present invention includes but is not limited to copper, tungsten or silver.
Preferably, the washing is washing with pure water.
Compared with the prior art, the invention has the following beneficial effects:
The plating film is a silver, palladium and gold plating layer, has no magnetism, does not influence signal high-frequency and high-speed transmission, can protect a conductive layer, provides good weldability, conductivity, corrosion resistance and friction resistance, and has lower production cost.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof. In the embodiment of the invention, the normal temperature is 25 ℃.
Example 1
The experimental substrate in this example was a copper-clad plate, and a test sample was prepared according to the process flow in table 1:
TABLE 1
Sequence number Name of procedure Temperature/. Degree.C Time/min
1 Deoiling 40 4
2 Pure water washing Normal temperature 0.5
3 Microetching 25 2
4 Pure water washing Normal temperature 0.5
5 Presoaking 40 1
6 Preparation of silver layer 50 3
7 Pure water washing Normal temperature 0.5
8 Preparation of palladium layer 52 10
9 Pure water washing Normal temperature 0.5
10 Preparation of gold layer 80 8
11 Pure water washing Normal temperature 0.5
Table 1 process flow 6 the process of preparing the silver layer is: placing the copper-clad plate obtained in the process flow 5 into a chemical silver solution to obtain a silver layer, wherein the pH value of the chemical silver solution is 8.5, the concentration of silver ammonia complex ions in the chemical silver solution is 3g/L, the concentration of triamine citrate is 10g/L, the concentration of glycine is 8g/L, and the concentration of citric acid is 10g/L;
Table 1 process flow 8 the palladium layer was prepared as follows: placing the product obtained in the process flow 7 into a chemical palladium solution to obtain a palladium layer, wherein the pH of the chemical palladium solution is 7, the concentration of palladium sulfate in the chemical palladium solution is 3g/L, the concentration of sodium ethylenediamine tetraacetate is 12g/L, the concentration of sodium citrate is 10g/L, the concentration of formic acid is 15g/L, the concentration of bismuth nitrate is 2mg/L, and the concentration of boric acid is 1g/L;
Table 1 process flow 10 the process of preparing the gold layer is: and (3) placing the product obtained in the process flow 9 in a chemical gold solution to obtain a gold layer, wherein the pH value of the chemical gold solution is 6.5, the concentration of gold potassium cyanide in the chemical gold solution is 3g/L, the concentration of acetohydroxamic acid is 15g/L, the concentration of lanthanum sulfate is 12mg/L, the concentration of 2, 2-dipyridylamine is 3mg/L, and the concentration of 2-morpholinoethanesulfonic acid is 10g/L.
Example 2
The experimental substrate in this example was a copper-clad plate, and a test sample was prepared according to the process flow in table 2:
TABLE 2
Sequence number Name of procedure Temperature/. Degree.C Time/min
1 Deoiling 35 5
2 Pure water washing Normal temperature 0.5
3 Microetching 23 2
4 Pure water washing Normal temperature 0.5
5 Presoaking 35 1
6 Preparation of silver layer 40 4
7 Pure water washing Normal temperature 0.5
8 Preparation of palladium layer 40 15
9 Pure water washing Normal temperature 0.5
10 Preparation of gold layer 70 8
11 Pure water washing Normal temperature 0.5
Table 2 process flow 6 the process of preparing the silver layer is: placing the copper-clad plate obtained in the process flow 5 into a chemical silver solution to obtain a silver layer, wherein the pH value of the chemical silver solution is 9, the concentration of silver sulfite complex ions in the chemical silver solution is 5g/L, the concentration of ammonium phosphate is 20g/L, the concentration of alpha-alanine is 20g/L, and the concentration of sulfosalicylic acid is 20g/L;
Table 2 process flow 8 the palladium layer was prepared as follows: placing the product obtained in the process flow 7 in a chemical palladium solution to obtain a palladium layer, wherein the pH of the chemical palladium solution is 6.5, the concentration of palladium chloride in the chemical palladium solution is 5g/L, the concentration of ethylenediamine is 20g/L, the concentration of succinic acid is 25g/L, the concentration of ascorbic acid is 25g/L, the concentration of thiourea is 5mg/L, and the concentration of sodium dihydrogen phosphate is 5g/L;
Table 2 process flow 10 the process of preparing the gold layer is: and (3) placing the product obtained in the process flow 9 into a chemical gold solution to obtain a gold layer, wherein the pH value of the chemical gold solution is 6, the concentration of gold potassium citrate in the chemical gold solution is 5g/L, the concentration of the benzalkonium hydroxide is 20g/L, the concentration of cerium sulfate is 25mg/L, the concentration of 2, 4-lutidine is 5mg/L, and the concentration of a citric acid-sodium citrate buffer solution is 25g/L.
Example 3
The experimental substrate in this example was a copper-clad plate, and a test sample was prepared according to the process flow in table 3:
TABLE 3 Table 3
Sequence number Name of procedure Temperature/. Degree.C Time/min
1 Deoiling 45 3
2 Pure water washing Normal temperature 0.5
3 Microetching 27 1
4 Pure water washing Normal temperature 0.5
5 Presoaking 45 1
6 Preparation of silver layer 70 2
7 Pure water washing Normal temperature 0.5
8 Preparation of palladium layer 70 4
9 Pure water washing Normal temperature 0.5
10 Preparation of gold layer 80 20
11 Pure water washing Normal temperature 0.5
Table 3 process flow 6 the process of preparing the silver layer is: placing the copper-clad plate obtained in the process flow 5 into a chemical silver solution to obtain a silver layer, wherein the pH value of the chemical silver solution is 8, the concentration of silver sulfite complex ions in the chemical silver solution is 0.5g/L, the concentration of ammonium acetate is 1g/L, the concentration of cystine is 1g/L, and the concentration of glucose is 1g/L;
Table 3 process flow 8 the palladium layer was prepared as follows: placing the product obtained in the process flow 7 in a chemical palladium solution to obtain a palladium layer, wherein the pH of the chemical palladium solution is 8, the concentration of dichlorotetraammine palladium in the chemical palladium solution is 0.1g/L, the concentration of ethylamine is 5g/L, the concentration of oxalic acid is 5g/L, the concentration of dimethylamine borane is 1g/L, the concentration of 2-mercaptobenzothiophene is 0.1mg/L, and the concentration of disodium hydrogen phosphate is 0.5g/L;
Table 3 process flow 10 the process of preparing the gold layer is: and (3) placing the product obtained in the process flow 9 in a chemical gold solution to obtain a gold layer, wherein the pH of the chemical gold solution is 7, the concentration of gold chloride in the chemical gold solution is 0.1g/L, the concentration of salicylic hydroxamic acid is 5g/L, the concentration of thallium sulfate is 1mg/L, the concentration of pyridine-2, 3 dihydroxyl is 0.1mg/L, and the concentration of bis (2-hydroxyethylamino) trimethylol methane is 1g/L.
Comparative example 1
A nickel layer, a palladium layer and a gold layer were deposited on the experimental substrate in example 1, the thicknesses of the palladium layer and the gold layer being the same as in example 1, and the thickness of the nickel layer being the same as that of the silver layer in example 1.
Performance testing
The following performance tests were carried out on the products obtained in each example and comparative example:
(1) Coating thickness by using an X-RAY thickness gauge;
(2) Passing through 255 ℃ lead-free tin furnace, and testing tin loading rate;
(3) Using 3M-610 adhesive tape for adhesion test, wherein the phenomenon of plating is not found to be excellent, and the phenomenon of plating is found to be poor;
(4) Testing the tension value of the gold thread after the gold thread bonding machine is used for wire bonding;
(5) 48H salt spray test was performed.
The performance test results are shown in table 4:
TABLE 4 Table 4
As can be seen from Table 4 of the present invention, the coating structure obtained in the examples of the present invention meets the ICP standard. Comparative example 1 has inferior performance to example 1, and it can be seen that the substitution of the nickel layer with the silver layer can effectively reduce the surface roughness and improve the signal insertion loss capability.
The present invention is described in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e., it does not mean that the present invention must be practiced depending on the above detailed methods. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.

Claims (22)

1. The coating structure is characterized by comprising a silver layer, a palladium layer and a gold layer which are sequentially arranged on a conductive layer; the conductive layer comprises copper and/or tungsten;
the thickness of the silver layer is 0.2-0.4 mu m;
the thickness of the palladium layer is 0.05-0.2 mu m;
the thickness of the gold layer is 0.05-0.2 mu m;
The coating structure is prepared by the following method, which comprises the following steps: sequentially preparing a silver layer, a palladium layer and a gold layer on the conductive layer to obtain a film coating structure;
The preparation method of the silver layer comprises the following steps: placing the conductive layer in a chemical silver solution to obtain a conductive layer with a silver layer covered on the surface, wherein the chemical silver solution comprises silver ions or complex silver ions, the chemical silver solution also comprises an amine complexing agent, an amino complexing agent and a polyhydroxy acid complexing agent, the pH value of the chemical silver solution is 8.0-9.0, the temperature of the chemical silver solution is 40-70 ℃, the concentration of the silver ions or the complex silver ions in the chemical silver solution is 0.5-5 g/L, the concentration of the amine complexing agent is 1-20 g/L, the concentration of the amino complexing agent is 1-20 g/L, and the concentration of the polyhydroxy acid complexing agent is 1-20 g/L;
The time for placing the conductive layer in the chemical silver solution is 2-4 min;
The preparation method of the palladium layer comprises the following steps: placing the conductive layer with the surface covered with the silver layer in a chemical palladium solution to obtain a pre-product, wherein the palladium layer in the pre-product is covered on the surface of the silver layer, the pH value of the chemical palladium solution is 7.0-8.0, the temperature of the chemical palladium solution is 40-70 ℃, and the time for placing the conductive layer with the surface covered with the silver layer in the chemical palladium solution is 4-15 min;
The chemical palladium solution comprises palladium salt, main complexing agent, auxiliary complexing agent, reducing agent, first stabilizer and first pH buffer, wherein the concentration of the palladium salt in the chemical palladium solution is 0.1-5 g/L, the main complexing agent is amino compound, the concentration of the main complexing agent is 5-20 g/L, the auxiliary complexing agent comprises any one or combination of at least two of sodium citrate, acrylic acid, succinic acid, oxalic acid and malic acid, the concentration of the auxiliary complexing agent is 5-25 g/L, the concentration of the reducing agent is 1-25 g/L, the first stabilizer comprises any one or combination of at least two of bismuth nitrate, thiourea, 4-dimethylaminopyridine and 2-mercaptobenzothiophene, the concentration of the first stabilizer is 0.1-5 mg/L, the first pH buffer comprises any one or combination of at least two of borax, boric acid, sodium dihydrogen phosphate and disodium hydrogen phosphate, and the concentration of the first pH buffer is 0.5-5 g/L;
the preparation method of the gold layer comprises the following steps: placing the pre-product in a chemical gold solution to obtain a coating structure;
The pH value of the chemical gold solution is 6.0-7.0, the temperature of the chemical gold solution is 70-80 ℃, and the time for placing the pre-product in the chemical gold solution is 0.5-20 min;
the chemical gold solution comprises gold salt, complexing agent, accelerator, second stabilizer and second pH buffer; in the chemical gold solution, the concentration of gold salt is 0.1-5 g/L, the concentration of complexing agent is 5-20 g/L, the concentration of accelerator is 1-25 mg/L, the second stabilizer comprises any one or combination of at least two of 2, 2-dipyridylamine, 2, 4-lutidine, 2, 4-dimethylpiperidine and pyridine-2, 3-dihydroxyacid, the concentration of the second stabilizer is 0.1-5 mg/L, the second pH buffer is any one or combination of at least two of 2-morpholinoethanesulfonic acid, bis (2-hydroxyethylamino) trimethylol methane, piperazine-1, 4-diethylsulfonic acid and citric acid-sodium citrate buffer, and the concentration of the second pH buffer is 1-25 g/L.
2. A method of making a coated structure according to claim 1, comprising: sequentially preparing a silver layer, a palladium layer and a gold layer on the conductive layer to obtain a film coating structure;
The preparation method of the silver layer comprises the following steps: placing the conductive layer in a chemical silver solution to obtain a conductive layer with a silver layer covered on the surface, wherein the chemical silver solution comprises silver ions or complex silver ions, the chemical silver solution also comprises an amine complexing agent, an amino complexing agent and a polyhydroxy acid complexing agent, the pH value of the chemical silver solution is 8.0-9.0, the temperature of the chemical silver solution is 40-70 ℃, the concentration of the silver ions or the complex silver ions in the chemical silver solution is 0.5-5 g/L, the concentration of the amine complexing agent is 1-20 g/L, the concentration of the amino complexing agent is 1-20 g/L, and the concentration of the polyhydroxy acid complexing agent is 1-20 g/L;
The time for placing the conductive layer in the chemical silver solution is 2-4 min;
The preparation method of the palladium layer comprises the following steps: placing the conductive layer with the surface covered with the silver layer in a chemical palladium solution to obtain a pre-product, wherein the palladium layer in the pre-product is covered on the surface of the silver layer, the pH value of the chemical palladium solution is 7.0-8.0, the temperature of the chemical palladium solution is 40-70 ℃, and the time for placing the conductive layer with the surface covered with the silver layer in the chemical palladium solution is 4-15 min;
The chemical palladium solution comprises palladium salt, main complexing agent, auxiliary complexing agent, reducing agent, first stabilizer and first pH buffer, wherein the concentration of the palladium salt in the chemical palladium solution is 0.1-5 g/L, the main complexing agent is amino compound, the concentration of the main complexing agent is 5-20 g/L, the auxiliary complexing agent comprises any one or combination of at least two of sodium citrate, acrylic acid, succinic acid, oxalic acid and malic acid, the concentration of the auxiliary complexing agent is 5-25 g/L, the concentration of the reducing agent is 1-25 g/L, the first stabilizer comprises any one or combination of at least two of bismuth nitrate, thiourea, 4-dimethylaminopyridine and 2-mercaptobenzothiophene, the concentration of the first stabilizer is 0.1-5 mg/L, the first pH buffer comprises any one or combination of at least two of borax, boric acid, sodium dihydrogen phosphate and disodium hydrogen phosphate, and the concentration of the first pH buffer is 0.5-5 g/L;
the preparation method of the gold layer comprises the following steps: placing the pre-product in a chemical gold solution to obtain a coating structure;
The pH value of the chemical gold solution is 6.0-7.0, the temperature of the chemical gold solution is 70-80 ℃, and the time for placing the pre-product in the chemical gold solution is 0.5-20 min;
The chemical gold solution comprises gold salt, complexing agent, accelerator, second stabilizer and second pH buffer; in the chemical gold solution, the concentration of gold salt is 0.1-5 g/L, the complexing agent comprises any one or a combination of at least two of acetohydroxamic acid, benzohydroxamic acid, salicylhydroxamic acid and acetohydroxamic acid, the concentration of the complexing agent is 5-20 g/L, the accelerator comprises any one or a combination of at least two of lanthanum sulfate, cerium sulfate and thallium sulfate, the concentration of the accelerator is 1-25 mg/L, the second stabilizer comprises any one or a combination of at least two of 2, 2-bipyridylamine, 2, 4-dimethylpyridine, 2, 4-dimethylpiperidine and pyridine-2, 3-dihydroxyacid, the concentration of the second stabilizer is 0.1-5 mg/L, the second pH buffer is any one or a combination of at least two of 2-morpholinoethanesulfonic acid, bis (2-hydroxyethylamino) trimethylol methane, piperazine-1, 4-diethylsulfonic acid and citric acid-buffer, and the concentration of the second buffer is 1-25 g/L.
3. The method of claim 2, further comprising a washing process after the silver layer is prepared on the conductive layer.
4.A method according to claim 3, wherein the washing is performed with pure water.
5. The method of claim 2, wherein the silver ion or complex silver ion comprises any one or a combination of at least two of a silver ammine complex ion, a silver sulfite complex ion, and a silver halide complex ion.
6. The method of claim 2, wherein the amine complexing agent comprises any one or a combination of at least two of ammonia, triamine citrate, ammonium phosphate, ammonium sulfate, ammonium nitrate, ammonium acetate, ammonium ethylene diamine carbonate, diethylenetriamine, aminopyridine of triethylenetetramine, aniline, and phenylenediamine.
7. The method of claim 2, wherein the amino complexing agent comprises any one or a combination of at least two of glycine, alpha-alanine, beta-alanine, cystine, ethylenediamine tetraacetic acid, aspartic acid, glutamic acid, sulfamic acid nitrilotriacetic acid, and aromatic cyclic amino acids.
8. The method of claim 2, wherein the polyhydroxy acid complexing agent comprises any one or a combination of at least two of an acid, an alkali metal salt of the acid, and an ammonium salt of the acid.
9. The method of claim 8, wherein the acid is any one or a combination of at least two of citric acid, tartaric acid, gluconic acid, malic acid, lactic acid, 1-hydroxy-ethylidene-1, 1-diphosphate, sulfosalicylic acid, and phthalic acid.
10. The method of claim 2, wherein the method of preparing the palladium layer further comprises a washing process after obtaining the pre-product.
11. The method of claim 10, wherein the washing is with pure water.
12. The method of claim 2, wherein the chemical palladium solution consists of palladium ions or palladium complex ions, a primary complexing agent, a secondary complexing agent, a reducing agent, a first stabilizing agent, and a first pH buffer.
13. The method of claim 2, wherein the palladium salt comprises any one or a combination of at least two of palladium sulfate, palladium chloride, ammonium palladium chloride, tetra-ammine palladium dichloride, and ammine palladium sulfate.
14. The method of claim 2, wherein the primary complexing agent comprises any one or a combination of at least two of aqueous ammonia, ethylenediamine, ethylamine, and sodium ethylenediamine tetraacetate.
15. The method of claim 2, wherein the reducing agent comprises any one or a combination of at least two of formic acid, hypophosphite, ascorbic acid, and dimethylamine borane.
16. The method of claim 2, further comprising a washing and drying process after the coated structure is obtained.
17. The method of claim 16, wherein the washing is with pure water.
18. The method of claim 16, wherein the temperature of the drying is 60 to 90 ℃.
19. The method of claim 2, wherein the electroless gold solution is comprised of a gold salt, a complexing agent, an accelerator, a second stabilizer, and a second pH buffer.
20. The method of claim 19, wherein the gold salt comprises any one or a combination of at least two of potassium gold cyanide, potassium gold citrate, gold chloride, and a hydrate of tetrachloroic acid.
21. The method of claim 2, wherein the conductive layer further comprises a degreasing, washing and microetching process prior to preparing the silver layer.
22. The method of claim 21, wherein the washing is with pure water.
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