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Apr 26, 2022 View: 113
What Are The Porosity Test Methods For PCB Gold Plating?
1 Introduction
Electrical and electronic products and devices are used in a variety of environmental conditions, and their connections are
prone to corrosion when exposed to the air, and are usually protected by surface gold plating. However, the international
gold price keeps rising. In 2008, the international gold price exceeded the integer mark of 1,000 US dollars. The rise in the
gold price further aggravated the production cost of printed circuit board manufacturers, and reduced the thickness of the
gold-plated layer without affecting its performance. R&D focus in the process.
While reducing the thickness of the gold-plated layer, it is necessary to meet the characteristics of anti-oxidation, high
solderability, high conductivity and high heat dissipation of the surface plating of the printed circuit board pads. The
technologies used are: organic solderability protective coating ( OrganicSolderabilityPreservatives OSP), electroless nickel
gold and electroplated nickel gold surface treatment.
The disadvantage of the organic solderability protective coating (OSP) process is that the protective film formed is extremely
thin and easily scratched (or scratched), which must be carefully operated and op-amped. At the same time, the OSP film
that has undergone multiple high-temperature soldering processes may be discolored or cracked, affecting solderability and
reliability. The thickness of the transparent OSP layer is not easy to measure, and the degree of coverage is not easy to see,
which makes it difficult for upstream buyers to evaluate the quality stability of these aspects.
Electroless nickel-gold or electro-nickel-gold surface treatment can make the surface of the printed circuit board pads very
flat and have good solderability. Secondly, due to the chemical inertness of gold in the normal environment, it can protect the
surface of the PCB pad from oxidation for a long period of time, and has the resistance to environmental corrosion and
excellent electrical properties that other surface treatment processes do not have. At the same time, the wear resistance
during plugging and unplugging is improved, the contact resistance is reduced, and the connection reliability is improved.
Since there are still some problems in domestic gold plating process and material processing, even after the OSP process,
there are still micropores on the surface of the gold plating layer. Therefore, it is of great practical significance to use how to
detect and control the quality of gold plating. Porosity is an important indicator to characterize the continuity of the nickel-
gold surface coating.
This paper analyzes the commonly used porosity inspection methods, and studies a new method for inspecting the porosity
of the gold-plated layer by taking the PCB pad samples that have undergone nickel-gold electroplating process and OSP
process as an example.
2. Commonly used porosity testing methods[1][2][3]
At present, the detection methods for the surface porosity of gold coatings are mainly divided into three categories:
①Gas exposure method;
② Electrolytic imaging test method;
③ Salt spray test. In the national standards GB/T17720-1999 (Review of the porosity test of metal covering layers),
GB/T4677-2002 (Test methods for printed boards), GB/T19351-2003 (Inspection of the porosity of metal covering layers on
metal substrates of metal covering layers) The porosity test method of the nickel-gold coating on the copper substrate is
specified in detail in the nitric acid vapor test).
①Gas exposure method
The gases used in this method are mainly sulfur dioxide, hydrogen sulfide, chlorine, nitric acid vapor, etc. It has high
requirements on test reagents, test equipment and test environment, and takes too long, and the gases used are all strongly
irritating and toxic, which can cause serious pollution to the atmosphere and pose safety hazards to the test operators. The
inspection result is to calculate the porosity by observing the number of rust spots and the degree of corrosion through a
low-power optical microscope, and the accuracy is greatly affected by the operator. Neither the usability of this test method
nor the reliability of the test results is high.
② Electrolytic imaging test method
This method mainly includes acrylamide electrolysis test, diacetyl oxime paper electrolysis phenomenon test, and
cyclohexanedione dioxime paper electrolysis phenomenon test. This method is simple to operate, and the test results are
less affected by operators. The disadvantage is that special instruments are required, and the test paper and developer
need to be specially prepared, and the detection operation involving gold, palladium, rhodium and other coatings on nickel
coatings is a toxic operation, so only a few printed board manufacturers use it.
③Salt spray test
This method mainly uses sodium chloride solution to spray continuously for a long time at a certain temperature. This
method is simple to operate, but the disadvantage is that it requires special instruments, takes too long, and is not easy to
accurately calculate the porosity. At present, most printed board manufacturers use this method to qualitatively evaluate the
coating quality.
3. Porosity test experiment [4]
3.1 Preparation before inspection
(1) Take a single piece of PCB finished board that has undergone electroplating nickel-gold process and OSP process as a
sample, and each whole board is not less than three single pieces. The sample should have exposed plating, such as gold
fingers, ground copper, pads, etc., and use ethanol to clean the surface to remove oil.
(2) Make a grid with scale that can be placed in a low-power optical microscope. The specific method: design a circular film
negative with a diameter of 23mm and a line width of 0.1mm. The grid line width is 0.1mm, and the scales are marked on the
four corners of the grid. The scale interval is 0.1mm, and the scale line width is 0.1mm. As shown in Figure-1, install the
circular grid under the eyepiece of a 20X optical microscope.
(3) Use rubber or wood blocks to make a bevel. Its dimensions are 5mm high, 25mm long, 15mm wide, and the inclination
angle tanα is 0.2.
3.2 Inspection solution composition and preparation
Detection solution Base metal or underlying metal plating
Ingredient name Ingredient content
HCl 2%~2.7% Copper, Nickel Nickel/Gold
NaCl 0.5~2.0%
Penetrating agent 0.02%~0.2%
Detect solution base metal or underlying metal coating
Ingredient name Ingredient content
HCl 2%~2.7% copper, nickel nickel/gold
NaCl 0.5~2.0%
Penetrant 0.02%~0.2%
Table-1 Solution composition
Detection solution Base metal or underlying metal plating
Ingredient name Ingredient content
HCl 2%~2.7% Copper, Nickel Nickel/Gold
NaCl 0.5~2.0%
Penetrating agent 0.02%~0.2%
The penetrant is a compounding agent containing one or more of the following surfactants: fatty alcohol polyoxyethylene
(5~6) ether, fatty acid polyoxyethylene ether, sodium alkylnaphthalenesulfonate, dibutylnaphthalenesulfonate Sodium and
Sodium Butylnaphthalene Sulfonate, etc. The role of the penetrant enhances the penetration of the solution and improves
the degree of contact between the inspection solution and the coating.
Preparation of test solution:
Add 100ml of deionized water to a 250ml volumetric flask, measure 11.77~15.88ml of 36% concentrated HCl, mix well, add
NaCl, then add 0.50~5.00ml of 10% penetrant, and add deionized water after complete dissolution to the tick mark. Both HCl
and NaCl were of analytical grade.
3.3 Inspection steps
(1) Control the temperature at 21°C-24°C, immerse the sample in the solution, keep it still for 5-8 minutes, take it out and
absorb the water with absorbent paper.
(2) Put the sample on the inclined plane and observe it with a 20X optical microscope. Move the sample to avoid the edge of
the coating and observe the pores.
(3) Calculate the porosity: select the continuous grid as the observation area, and the total observation area is not less than
50% of the total coating area, count the number of pores, and calculate the porosity (number of pores/cm2).
Pore calculations are performed according to Table-2, and the diameter of the pores is measured by the scale on the grid.
Pore size calculation of the number of pores
Maximum diameter≤0.05mm 0
0.05mm< maximum diameter<0.1 mm 1
0.1mm≤ maximum diameter <0.2mm 2
Maximum diameter ≥ 0.2mm 5
Pore size Calculate the number of pores
Maximum diameter≤0.05mm 0
0.05mm< maximum diameter<0.1 mm 1
0.1mm≤ maximum diameter <0.2mm 2
Maximum diameter ≥ 0.2mm 5
Pore size Calculate the number of pores
Maximum diameter≤0.05mm 0
0.05mm< maximum diameter<0.1 mm 1
0.1mm≤ maximum diameter <0.2mm 2
Maximum diameter ≥ 0.2mm 5
4. Check the reaction mechanism between the solution and the coating
(1) Reaction mechanism
In order to increase the flexibility of the product, the flexible printed circuit board manufacturer has a very thin nickel-plated
gold layer. Generally, the nickel layer is about 1.5μm, and the gold layer is 0.02-0.1μm. The gold-plated layer is extremely
thin. In order to achieve the effective coverage and protection of the gold-plated layer, an organic solderability protective
coating (OSP) is used as a capping agent for the gold-plated layer in production. The protective coating is an extremely thin
protective film that does not react with hydrochloric acid.
The reaction mechanism for determining the porosity is that in an acidic solution, hydrochloric acid penetrates into the nickel-
plated layer through the pores not covered by the gold-plated layer under the action of the penetrant, and undergoes a redox
reaction with the nickel-plated layer, and the nickel is dissolved, leaving fine needles. The number of micropores can be
observed and counted under a low magnification microscope. The reaction mechanism is as follows:
Ni +2HCl → NiCl2 + H2↑
Sodium chloride provides an electrolyte environment for the system, metallic nickel acts as the negative electrode of the
corrosive primary battery, and gold acts as the positive electrode of the corrosive primary battery, forming a corrosive
primary battery and accelerating the originally existing pinhole corrosion.
Corrosion of the galvanic electrode reaction is as follows:
Primary battery reaction negative electrode: Ni -2e→Ni2+
The positive electrode of the primary battery reaction: 2H+ +2e→H2
(2) The reason why the sample is placed on the inclined plane to observe
Since hydrochloric acid does not react with copper, when the nickel in the pinhole is dissolved, the bottom layer is copper
layer. When light is irradiated, the gold surface reflects light, and the hole can also reflect light, thereby weakening the
distinction between the hole and the gold surface. Under the optical microscope Pores cannot be distinguished. Therefore,
the tilt angle is used to increase the reflection discrimination,
(3) Check the effect of each component of the solution and the influence of temperature and time
The role of HCl: check the main components of the solution, provide an acidic environment, and react with bare nickel. The
role of NaCl: provide ions to accelerate pinhole corrosion. The role of penetrant: as an acid-resistant penetrant, it can
enhance the penetration of the solution, improve the contact between the inspection solution and the coating, and promote
the reaction. Temperature: The temperature has a significant effect on the reaction rate. If the temperature is too high, the
reaction will be rapid, and the pores will expand and finally lead to the dissolution of the nickel layer and the detachment of
the gold layer. The appropriate temperature should be selected according to the production conditions. Time: The soaking
time has a great influence on the pores. The longer the time is, the more nickel is dissolved, and the larger the pores are.
However, if the time is too long, the nickel layer will be completely dissolved and the gold layer will fall off. Generally, 5min is
appropriate.
5. Analysis of porosity test results
There are different exposed gold-plated areas on a sample, and the flattening fingers, plug fingers and grounding copper are
tested separately in this paper.
5.1 Comparison of samples before and after treatment with test solution (taking unqualified products as an example)
The metallographic pictures before and after the test solution treatment are obviously different. The hydrochloric acid in the
test solution penetrates into the nickel-plated layer through the pores not covered by the gold-plated layer under the action of
the penetrant, and a primary battery reaction occurs. As a result, the pores are enlarged and can be observed under a low
magnification optical microscope.
5.2 Influence of temperature on test results
Under the conditions of temperature of 22 ℃ and 30 ℃, the qualified and unqualified products are processed by the
inspection solution. Temperature has little effect on the test results, so the test solution can be used in a wide temperature
range.
Through the comparison of qualified and unqualified products, it can be seen that the test solution can also distinguish
qualified and unqualified products well, as shown in Figure-6. The porosity is calculated by weighting the pore diameter.
According to a large number of experiments by our company, it is calculated that the porosity is less than or equal to 5
pieces/mm2 as a qualified product (for reference only).
6. Summary
(1) The main components of the test solution are hydrochloric acid, sodium chloride and penetrant, which do not react with
the organic solderability protective coating. The measured porosity is the porosity after capping, which truly characterizes the
quality of the surface coating.
(2) Using the solution immersion method, the observation uses a low-power optical microscope, and the tiny pores on the
thin gold coating can be easily observed by using the inclined plane. A grid film with a scale is placed in the microscope, and
the pore size is weighted, which facilitates the calculation of porosity.
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