CN109112506B - Activation inhibitor for production of fine line products and preparation method thereof - Google Patents
Activation inhibitor for production of fine line products and preparation method thereof Download PDFInfo
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- CN109112506B CN109112506B CN201811085748.0A CN201811085748A CN109112506B CN 109112506 B CN109112506 B CN 109112506B CN 201811085748 A CN201811085748 A CN 201811085748A CN 109112506 B CN109112506 B CN 109112506B
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- activation inhibitor
- palladium salt
- propane sulfonate
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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
- C23C18/1851—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
- C23C18/1879—Use of metal, e.g. activation, sensitisation with noble metals
Abstract
The invention discloses an activation inhibitor for production of fine line products and a preparation method thereof. The activation inhibitor comprises 2 to 10 percent of sulfuric acid, 0.001 to 0.008 percent of palladium salt, 0.003 to 0.012 percent of pyridinium hydroxy propane sulfonate and the balance of water. The activating solution can be used for producing circuit board products with the distance of 15um/15um in a mass production mode, the service life of the bath solution is long, no quality risk exists, and the operation and management are convenient.
Description
Technical Field
The invention relates to the technical field of fine line product production, in particular to an activation inhibitor for fine line product production and a preparation method thereof.
Background
In the traditional electroless chemical nickel gold (or electroless chemical nickel palladium gold, electroless chemical palladium gold) process, palladium sulfate or palladium chloride is generally adopted to carry out activation treatment on the circuit board, and when the method is used for producing products with the line width and the line distance of less than 50um/50um, seepage plating, residual gold, connecting lines and other abnormalities are easy to occur, so that the products are scrapped.
Manufacturers generally reduce the reject ratio of products by reducing the contact time between the circuit board and chemicals, reducing the reaction temperature, reducing the palladium content in the activating solution, prolonging the cleaning time, reducing the electroless nickel temperature, and the like, but such abnormalities cannot be completely avoided.
Therefore, there is a need for an activation inhibitor capable of inhibiting the reaction rate of Pb2+ ions and a preparation method thereof.
Disclosure of Invention
The invention provides an activation inhibitor for production of fine line products and a preparation method thereof, aiming at solving the problem that products are scrapped due to the fact that seepage plating, residual gold, connection and other abnormalities are easy to occur when products with line width and line distance of below 50um/50um are produced by the method in the prior art by adopting palladium sulfate or palladium chloride to carry out activation treatment on circuit boards.
The technical scheme adopted by the invention to achieve the aim is as follows: an activation inhibitor for production of fine line products is prepared from the following raw materials in percentage by weight:
2 to 10 percent of sulfuric acid, 0.001 to 0.008 percent of palladium salt, 0.003 to 0.012 percent of pyridinium hydroxy propane sulfonate and the balance of water.
In some embodiments, the activation inhibitor is prepared from the following raw materials in percentage by weight:
2 to 9 percent of sulfuric acid, 0.002 to 0.008 percent of palladium salt, 0.004 to 0.012 percent of pyridinium hydroxy propane sulfonate and the balance of water.
In some embodiments, the activation inhibitor is prepared from the following raw materials in percentage by weight:
3 to 7 percent of sulfuric acid, 0.002 to 0.006 percent of palladium salt, 0.004 to 0.01 percent of pyridinium hydroxy propane sulfonate and the balance of water.
In some embodiments, the palladium salt is palladium sulfate or palladium hydrochloride.
The invention also provides a preparation method of the activation inhibitor, which is characterized by comprising the following steps:
step 1: weighing a proper amount of water, sulfuric acid, palladium salt and pyridinium hydroxy propane sulfonate according to the proportion;
step 2, adding the sulfuric acid weighed in the step 1 into the water weighed in the step 1 for circulation, and cooling the solution;
step 3, adding the palladium salt and the pyridinium hydroxy propane sulfonate in the step 1 into the mixed solution in the step 2 for circulation to form the solution;
and 3, adding the palladium salt and the pyridinium hydroxy propane sulfonate sequentially or simultaneously.
In some embodiments, the step 2 requires a cycle of more than 4 h.
In some embodiments, the solution in step 2 needs to be cooled to 20-30 degrees celsius.
In some embodiments, a cycle of 2h is required in step 3.
The invention has the beneficial effects that: compared with the prior art, the invention comprises 2 to 10 percent of sulfuric acid, 0.001 to 0.008 percent of palladium salt, 0.003 to 0.012 percent of pyridinium hydroxy propane sulfonate and the balance of water. The activating solution can be used for producing circuit board products with the distance of 15um/15um in a mass production mode, the service life of the bath solution is long, no quality risk exists, and the operation and management are convenient.
Drawings
FIG. 1 is a schematic diagram of a conventional activation reaction in a nickel-gold process;
FIG. 2 is a schematic diagram of an activation reaction according to the present invention;
FIG. 3 is an enlarged view of the surface structure of a product produced by a conventional process;
fig. 4 is an enlarged view of the surface structure of the product produced by the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
As shown in fig. 1 to 4, the invention provides an activation inhibitor for the production of fine line products, which is prepared from the following raw materials in percentage by weight:
2 to 10 percent of sulfuric acid, 0.001 to 0.008 percent of palladium salt, 0.003 to 0.012 percent of pyridinium hydroxy propane sulfonate and the balance of water.
In some embodiments, the activation inhibitor is prepared from the following raw materials in percentage by weight:
2 to 9 percent of sulfuric acid, 0.002 to 0.008 percent of palladium salt, 0.004 to 0.012 percent of pyridinium hydroxy propane sulfonate and the balance of water.
In some embodiments, the activation inhibitor is prepared from the following raw materials in percentage by weight:
3 to 7 percent of sulfuric acid, 0.002 to 0.006 percent of palladium salt, 0.004 to 0.01 percent of pyridinium hydroxy propane sulfonate and the balance of water.
In some embodiments, the palladium salt is palladium sulfate or palladium hydrochloride.
The invention also provides a preparation method of the activation inhibitor, which comprises the following steps:
step 1: weighing a proper amount of water, sulfuric acid, palladium salt and pyridinium hydroxy propane sulfonate according to the proportion;
step 2, adding the sulfuric acid weighed in the step 1 into the water weighed in the step 1 for circulation, and cooling the solution;
step 3, adding the palladium salt and the pyridinium hydroxy propane sulfonate in the step 1 into the mixed solution in the step 2 for circulation, and finally filtering to form the solution;
and 3, adding the palladium salt and the pyridinium hydroxy propane sulfonate sequentially or simultaneously.
In some embodiments, the step 2 requires a cycle of more than 4 h.
In some embodiments, the solution in step 2 needs to be cooled to 20-30 degrees celsius.
In some embodiments, a cycle of 2h is required in step 3.
Example 1
An activation inhibitor for production of fine line products is prepared from the following raw materials in percentage by weight:
2% of sulfuric acid, 0.001% of palladium salt, 0.003% of pyridinium hydroxy propane sulfonate and the balance of water.
In this embodiment, the palladium salt is palladium sulfate.
Example 2
A method of preparing the activation inhibitor of example 1, the method comprising:
step 1: weighing a proper amount of water, sulfuric acid, palladium salt and pyridinium hydroxy propane sulfonate according to the proportion;
step 2, adding the sulfuric acid weighed in the step 1 into the water weighed in the step 1 for circulation, and cooling the solution;
step 3, adding the palladium salt and the pyridinium hydroxy propane sulfonate in the step 1 into the mixed solution in the step 2 for circulation to form the solution;
and 3, adding the palladium salt and the pyridinium hydroxy propane sulfonate sequentially or simultaneously.
In this example, a cycle of 4h is required in step 2.
In this example, the solution in step 2 needs to be cooled to 20 degrees celsius.
In this example, a cycle of 2h is required in step 3.
Example 3
An activation inhibitor for production of fine line products is prepared from the following raw materials in percentage by weight:
10% of sulfuric acid, 0.008% of palladium salt, 0.012% of pyridinium hydroxy propane sulfonate and the balance of water.
In this embodiment, the palladium salt is palladium sulfate.
Example 4
A method of preparing the activation inhibitor of example 3, the method comprising:
step 1: weighing a proper amount of water, sulfuric acid, palladium salt and pyridinium hydroxy propane sulfonate according to the proportion;
step 2, adding the sulfuric acid weighed in the step 1 into the water weighed in the step 1 for circulation, and cooling the solution;
step 3, adding the palladium salt and the pyridinium hydroxy propane sulfonate in the step 1 into the mixed solution in the step 2 for circulation to form the solution;
and 3, adding the palladium salt and the pyridinium hydroxy propane sulfonate sequentially or simultaneously.
In this example, a cycle of 5h is required in step 2.
In this example, the solution in step 2 needs to be cooled to 30 degrees celsius.
In this example, a cycle of 2h is required in step 3.
Example 5
An activation inhibitor for production of fine line products is prepared from the following raw materials in percentage by weight:
6% of sulfuric acid, 0.005% of palladium salt, 0.008% of pyridinium hydroxy propane sulfonate and the balance of water.
In this embodiment, the palladium salt is palladium sulfate.
Example 6
A method of preparing the activation inhibitor of example 5, the method comprising:
step 1: weighing a proper amount of water, sulfuric acid, palladium salt and pyridinium hydroxy propane sulfonate according to the proportion;
step 2, adding the sulfuric acid weighed in the step 1 into the water weighed in the step 1 for circulation, and cooling the solution;
step 3, adding the palladium salt and the pyridinium hydroxy propane sulfonate in the step 1 into the mixed solution in the step 2 for circulation to form the solution;
and 3, adding the palladium salt and the pyridinium hydroxy propane sulfonate sequentially or simultaneously.
In this example, a loop of 6h is required in step 2.
In this example, the solution in step 2 needs to be cooled to 25 degrees celsius.
In this example, a cycle of 2h is required in step 3.
Example 7
An activation inhibitor for production of fine line products is prepared from the following raw materials in percentage by weight:
3% of sulfuric acid, 0.002% of palladium salt, 0.004% of pyridinium hydroxy propane sulfonate and the balance of water.
In this embodiment, the palladium salt is palladium sulfate.
Example 8
A method of preparing the activation inhibitor of example 7, the method comprising:
step 1: weighing a proper amount of water, sulfuric acid, palladium salt and pyridinium hydroxy propane sulfonate according to the proportion;
step 2, adding the sulfuric acid weighed in the step 1 into the water weighed in the step 1 for circulation, and cooling the solution;
step 3, adding the palladium salt and the pyridinium hydroxy propane sulfonate in the step 1 into the mixed solution in the step 2 for circulation to form the solution;
and 3, adding the palladium salt and the pyridinium hydroxy propane sulfonate sequentially or simultaneously.
In this example, a cycle of 5.5h is required in step 2.
In this example, the solution in step 2 needs to be cooled to 20 degrees celsius.
In this example, a cycle of 2h is required in step 3.
Example 9
An activation inhibitor for production of fine line products is prepared from the following raw materials in percentage by weight:
7% of sulfuric acid, 0.006% of palladium salt, 0.01% of pyridinium hydroxy propane sulfonate and the balance of water.
In this embodiment, the palladium salt is palladium sulfate.
Example 10
A method of preparing the activation inhibitor of example 9, the method comprising:
step 1: weighing a proper amount of water, sulfuric acid, palladium salt and pyridinium hydroxy propane sulfonate according to the proportion;
step 2, adding the sulfuric acid weighed in the step 1 into the water weighed in the step 1 for circulation, and cooling the solution;
step 3, adding the palladium salt and the pyridinium hydroxy propane sulfonate in the step 1 into the mixed solution in the step 2 for circulation to form the solution;
and 3, adding the palladium salt and the pyridinium hydroxy propane sulfonate sequentially or simultaneously.
In this example, a cycle of 7h is required in step 2.
In this example, the solution in step 2 needs to be cooled to 20 degrees celsius.
In this example, a cycle of 2h is required in step 3.
Example 11
An activation inhibitor for production of fine line products is prepared from the following raw materials in percentage by weight:
5% of sulfuric acid, 0.004% of palladium salt, 0.007% of pyridinium hydroxy propane sulfonate and the balance of water.
In this embodiment, the palladium salt is palladium sulfate.
Example 12
A method of preparing the activation inhibitor of example 11, the method comprising:
step 1: weighing a proper amount of water, sulfuric acid, palladium salt and pyridinium hydroxy propane sulfonate according to the proportion;
step 2, adding the sulfuric acid weighed in the step 1 into the water weighed in the step 1 for circulation, and cooling the solution;
step 3, adding the palladium salt and the pyridinium hydroxy propane sulfonate in the step 1 into the mixed solution in the step 2 for circulation to form the solution;
and 3, adding the palladium salt and the pyridinium hydroxy propane sulfonate sequentially or simultaneously.
In this example, a cycle of 6.5h is required in step 2.
In this example, the solution in step 2 needs to be cooled to 30 degrees celsius.
In this example, a cycle of 2h is required in step 3.
In summary, the invention comprises 2 to 10 percent of sulfuric acid, 0.001 to 0.008 percent of palladium salt, 0.003 to 0.012 percent of pyridinium hydroxypropanesulfonate and the balance of water. The activating solution can be used for producing circuit board products with the distance of 15um/15um in a mass production mode, the service life of the bath solution is long, no quality risk exists, and the operation and management are convenient.
The above examples only show two embodiments of the present invention, and the description thereof is specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (8)
1. An activation inhibitor for production of fine line products is characterized by being prepared from the following raw materials in percentage by weight:
2 to 10 percent of sulfuric acid, 0.001 to 0.008 percent of palladium salt, 0.003 to 0.012 percent of pyridinium hydroxy propane sulfonate and the balance of water.
2. The activation inhibitor for the production of fine line products according to claim 1, wherein the activation inhibitor is prepared from the following raw materials in percentage by weight:
2 to 9 percent of sulfuric acid, 0.002 to 0.008 percent of palladium salt, 0.004 to 0.012 percent of pyridinium hydroxy propane sulfonate and the balance of water.
3. The activation inhibitor for the production of fine line products according to claim 2, wherein the activation inhibitor is prepared from the following raw materials in percentage by weight:
3 to 7 percent of sulfuric acid, 0.002 to 0.006 percent of palladium salt, 0.004 to 0.01 percent of pyridinium hydroxy propane sulfonate and the balance of water.
4. The activation inhibitor for use in the production of fine line products according to any one of claims 1 to 3, wherein the palladium salt is palladium sulfate or palladium hydrochloride.
5. A process for preparing an activation inhibitor according to any one of claims 1 to 4, comprising:
step 1: weighing a proper amount of water, sulfuric acid, palladium salt and pyridinium hydroxy propane sulfonate according to the proportion;
step 2, adding the sulfuric acid weighed in the step 1 into the water weighed in the step 1 for circulation, and cooling the solution;
step 3, adding the palladium salt and the pyridinium hydroxy propane sulfonate in the step 1 into the mixed solution in the step 2 for circulation to form the solution;
and 3, adding the palladium salt and the pyridinium hydroxy propane sulfonate sequentially or simultaneously.
6. The method for preparing an activation inhibitor according to claim 5, wherein the cycle of step 2 is required to be 4 hours or more.
7. The method for preparing an activation inhibitor according to claim 5, wherein the solution in the step 2 needs to be cooled to 20-30 ℃.
8. The method for preparing an activation inhibitor according to claim 5, wherein a cycle of 2 hours is required in the step 3.
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| GB836480A (en) * | 1957-01-15 | 1960-06-01 | Du Pont | Improvements in or relating to alloy plate |
| JP6620103B2 (en) * | 2014-09-04 | 2019-12-11 | 日本高純度化学株式会社 | Palladium plating solution and palladium film obtained using the same |
| CN104561943B (en) * | 2014-12-27 | 2017-05-10 | 广东致卓精密金属科技有限公司 | Chemical nickel-palladium alloy plating process for circuit boards |
| CN105695963B (en) * | 2016-04-27 | 2019-03-01 | 电子科技大学 | The end blocking method of minisize component pin |
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