Metallic coatings-Porosity tests-Humid sulfur (flowers of sulfur) test
Some standard content:
ICS 25. 220. 01
No. 1
National Standard of the People's Republic of China
GB/T 18179—2000
idt ISO 12687: 1996
Metallic coatings-Porosity testsHumid sulfur (flowers of sulfur) test2000-08-28 Issued
Implemented on 2001-01-01
Issued by the State Administration of Quality and Technical Supervision
TKAoNTKAca
GB/T 18179-2000
This standard is equivalent to the international standard IS012687:1996 (E>8 Jinni coating porosity test sulfur (sulfur flower) test) Appendix A and Appendix B of this standard are indicative appendices. This standard is proposed by the State Machinery Industry Bureau. This standard is under the jurisdiction of the National Technical Committee for the Promotion of Metal and Non-metallic Coating Standards. Drafting unit of this standard: Wuhan Institute of Materials Protection Drafters of this standard: Li Shun, Zhu Shasheng. TriKAoNiKAca
GB/T 18179—2000
ISO Foreword
ISO (International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of formulating international standards is mainly carried out through ISO technical committees. If a member body is interested in a subject determined by a technical committee, it has the right to submit a proposal to the committee. International governmental and non-governmental organizations in contact with ISO may also participate in this work. In all aspects of international electrotechnical standardization, ISO works closely with the International Electrotechnical Commission (IEC). The draft international standard formulated by the technical committee is first sent to the member groups for voting. At least 75% of the member groups participating in the voting according to the IS procedure must approve it before it can be published as an international standard. The international standard ISO 12687 was formulated by the SC7 Corrosion Testing Subcommittee of the ISO/TC107 Gold and Other Inorganic Coatings Technical Committee.
Appendices A and B of this international standard It is an appendix to the prompt. irKAONiKca
National Standard of the People's Republic of China
Metallic coatings-Porosity tests
Humid sulphur (hlowergof sulfur) test
Metallic cpatings-Porosity testsHumid sujfur (hlowergof sulfur)test1 Scope
This standard specifies the method of revealing
.
This method is particularly suitable for
palladium and its alloys.
GB/T 181792000
idt 1sO 12687: 1996
The test method is intended to show whether the interested layer meets the acceptable porosity level requirements set by the user, and whether the discontinuous and porous material of various single or red-colored covering layers such as steel, aluminum, tin, tin, aluminum, etc. that penetrate the single or multi-layer capping layer in the warm layer and reach the base of stainless steel, steel or alloy. SSEH
Users can use their experience to determine the degree of porosity test for cover layer porosity test according to the intended application. 2 Reference standards
Original rate specifications are generally based on the latest review of test methods (see Appendix 1 for reference) [1][2]
Metal and other inorganic coatings
See GB/T 17720 (Review of porosity test for metallic coatings) in the following standards. All standards are valid. GB/T 3138-1995
GB/T 6682—1992
GB/T 17720-1999
3 Definitions
This standard specifies the text. When this standard is released, the versions shown are all, by using the pages of this standard as the basis for ordering, you can use the latest version of this standard.
Parties should consider
using the following standards
Terminology for related processes (neg ISO 2079:1981 and ISO 2080.1981) and chemical
physics
Specifications and test methods (neg ISO
Review of laboratory water
rate test (eqv)).
This standard adopts the following definitions, except that
3.1 Physical corrosion product
GB/T 315
96:1987
0308:1995)
A chemical reaction product produced by the matrix that is ejected from a surface discontinuity. The chemical reaction products are generated during the test and can be easily detected after the test. They cannot be removed by graded air dust removal [see 10+-32]. 3.2 Discontinuity
Openings through the coating: typically holes or cracks in the short coating. They may also be caused by mechanical damage (e.g., scratches) or non-conductive impurities in the substrate material. 3.3 Measurement area
In this method, it refers to one or more surface areas where the detection holes exist. The measurement area should be marked on the workpiece paper or given by a suitably marked specimen.
3.4 Metallic coatings Metallic coatings are self-catalytic layers, chemical (non-electrolytic) plating, coatings, electroplating and thermal diffusion layers covering the substrate. The cover layer can be composed of a single metal layer or a combination of metal layers.
3.5 Pore
GB/T 181792000
A pore, typically a small hole with microscopic size, randomly distributed, and multi-shaped. The micropores penetrate the cover layer to the base coating or substrate.
3.6 Porosity
Cracks, discontinuities, micropores or paint damage in the cover layer that expose the base metal 3. Major surface Sigmificant surface The part or parts of the surface of the cover layer that are essential to the usability or function of the workpiece, or can become the precursor of detached products or discoloration films and affect the function of the workpiece. The major surface of many spot products is the same as the measurement area. 3.8 Tarnish film
The reaction product of copper or silver with oxygen or reducing agents (i.e., HS and sulfur vapor, but not SO, or other oxides of sulfur) which exists as a film or stain but does not clearly protrude from the surface of the metal finish (this is different from the isolated product) 3.9 Tarnish creepage
The rapid movement of the metal surface. The tarnish originates from micropores, cracks in the deposited layer or exposed areas of the substrate metal near the measured area (e.g., cut edges). Also called tarnish corrosion. 3.10 Underplate
The double deposit of metal between the substrate and the top layer. The friction of the underplate is usually greater than 1 um and there may be multiple underplates. 4.1.2.3 The test causes the substrate gold or underplate to react with sulfur vapor in a humid environment to form sulfides and oxides. These reaction products are exposed through discontinuities in the metal cover layer. The sulfides of silver and steel and the oxides of copper form dark or brown spots that are easily observed by the naked eye.
5 Summary of the Method
The specimen is suspended in a test container above the flower of sulfur (powder). The test container should be equipped with an air vent and have a controlled relative humidity and temperature. In this closed system, the sulfur vapor is always kept in a state of equilibrium with the flower of sulfur and isolates any exposed base metal or bottom coating, such as copper, aluminum alloy, silver or silver alloy exposed at the bottom of the micropores. Black or brown discoloration marks indicate the presence of pores. The test period is variable, depending on the degree of pore limitation to be revealed. This test involves a discoloration or oxidation (corrosion) reaction in which the corrosion products indicate the location of defects in the coating. The test shape or composition and chemical properties of the corrosion products are usually not similar to those in the natural environment or the use environment. Therefore, unless a correlation with use experience has been established in advance, this type of test is not recommended for environmental testing of product performance. 6 Reagents
6.1 Purity
The potassium hydroxide used in the test should be an analytically pure reagent.The test water shall be distilled water or deionized water with a conductivity of not more than 20 s/cm (compare with GB/T 6682). Commercial laboratory reagents shall be used. 6.2 Potassium nitrate solution and potassium nitrate solution are prepared by adding about 200 ml of potassium nitrate (KNO.) to about 200 ml of water (see 6.1). Note that the saturated solution is insoluble in potassium nitrate salt. This condition is necessary to achieve a constant humid atmosphere above the liquid. 6.3 Reagents: precipitated sulfur (flowers of sulfur), equipment 7.1 Test container GB/T 18179-2000 Use a transparent container made of glass or acrylic resin (or other materials not affected by sulfur and high humidity) of suitable size, for example, a desiccator with a capacity of about 10 L. The container should have a hole on the lid that can be tightened by the cold. The size of the hole should be large enough to insert the remote temperature and humidity sensor. There should also be a vent hole with a diameter of 1 to 4 mm on the plug. 7.2 Sample rack
The sample rack or hanger should be made of materials that are not affected by mercury and high humidity, such as glass, acrylic resin or polypropylene plastic. It should be placed so that the sample is at least 75 mm away from the wet extraction control solution (potassium phosphate solution) and sulfur (see 7.3), the sample is at least 25 mm away from the entire container, and the test ladder is at least 10 mm away from it and from other surfaces. Do not use the container partition as the main support, but it can be used as a lower support! The hanger and support should not cover more than 20% of the stirring area of the container so that the air convection in the container is not restricted during the test. 7.3 Glass sub-
A shallow stop made of glass or other material not affected by sulfur and high humidity with a diameter of about 150 mm is used to hold sulfur flowers. This III can be placed above the humidity control liquid with a block of material, or float on the liquid surface: the empty area of the surface should be large enough to ensure the humidity equilibrium condition in the container during the entire test.
7.4 Oven
Can maintain the temperature of 50℃±2℃ in the test container. 7.5 Thermometer or other temperature sensor
Can control the temperature in the test container at least within the range of 40℃±1℃ to 60℃±1℃ during the test. 7.6 Dielectric hygrometer
Has a remote sensing probe placed in the test container, and the humidity range of its test is 75%~95%RH7.7 Optical stereo microscope
The magnification is ×10. Its eyepiece contains a scale to measure the diameter of the color change. The scale should be calibrated for the magnification to be used.
7.8 Light source
Can be incandescent or fluorescent.
8 Sample preparation
The sample should be prevented from unnecessary movement. The sample should be moved with clamps, microscope test paper or clean soft cotton or nylon gloves. Before testing, use a 10x stereo microscope (see 7.7) to check whether there are foreign particles attached to the sample. If there are, remove them with clean, oil-free air: rinse the sample from which the attached particles have been removed with a solvent or a solvent containing no CFCs or other known ozone-depleting compounds, and then dry it with clean air: to accelerate drying, heat the sample in analytically pure methanol, ethanol, denatured alcohol or isopropanol.
The following procedures will help avoid the use of hydrogenated hydrocarbons: a) During each cleaning step, if there is a possibility of damage to the measurement area, the samples should be separated by this. b) Wash the sample in an ultrasonic cleaner for 5 min. Ultrasonic cleaning waves are hot (65~85) 2% alkaline (pH7-6pH10) detergent solution.
-) After ultrasonic cleaning, rinse the sample thoroughly with warm running water for not less than 5 s.d) Ultrasonic cleaning of the sample with freshly dissolved distilled water or deionized water (see 6.1) for 2 min to remove the last traces of detergent. e) The sample is placed in fresh analytically pure methanol, ethanol, denatured alcohol or isopropanol and stirred ultrasonically for not less than 303 to remove the moisture from the sample.
Remove the sample and air dry until the alcohol is completely evaporated. If a hair dryer is used to accelerate the drying, ensure that the air blown out is clean, oil-free and dry.
TTIKAONKACa
GB/T 18179—2000
After washing, do not touch the test area of the sample with your hands. Use a ×10 microscope to check if there are still foreign particles attached to the surface of the sample. If there are, repeat the above cleaning process. Since dirt (such as sensitive coating salt, gold fart crumbs, etc.) may falsely indicate porosity, it is extremely important to clean the sample surface. If the sample surface has an anti-discoloration layer or a lubricating layer or both, and their effectiveness in a reducing atmosphere is to be determined, the cleaning process can be omitted.
The preparation of conventional porosity test samples should enable the test area (i.e., the main surface) to be optimally exposed to the test environment. 9 Procedures 9.1 Equilibration of the Test Vessel During initial operation of the test, the test vessel (see 7.12) shall be equilibrated for at least 24 h before the first exposure of the specimens to the test chamber (see 9.2 of this section). Note: For all subsequent tests a) the test vessel shall be kept together with the test vessel (see 6.2). To ensure that no potassium crystals fall within 50 °C. While the equilibration is still in progress, add saturated acid-resistant egg solution (see saturated state) into the container, close the opening of the cover under room temperature (grease seal, cover the container! See 7.6), adjust the temperature to 55℃ (see 7.5) and measure the humidity. During the equilibrium process, open the container at appropriate times so that the temperature in the container reaches 100%.
d) Place the flowers of sulphur c
on top or directly on
e and cover again. Adjust the oven temperature. When the range is within
, it can be kept at 60℃.
Washing solution
Test container
About 20g/100m2 Add potassium nitrate) Insert the temperature of a thermometer or other temperature sensor and adjust the oven temperature appropriately. The ventilation port on the plug should not be sealed to prevent the relative humidity of the plug from approaching the semi-permeable glass blood (see 7.3) (If there are lumps of flowers of sulphur, they should be removed). Then place the glass blood on the potassium nitrate solution (see Figure 1). ||tt ||In the opening of the lid
the temperature of the instrument shop
is controlled
with ground seal (grease-free)
dryer
potassium nitrate falls
the spicy
of Mijishu
is very cold
the temperature in the container is measured for several hours, and the instrument must be stable, and the relative humidity is between 85% and 90%. There are electronic
separation and skin sensors
sample channel
Figure 1 Layout of typical test equipment
The test system described in this article can be repeatedly used for subsequent tests without replacing chemical reagents: as long as the chemical reagents do not intercept valuable products and contaminants, they can be stored for more than half a year. When the test system cools, the nitric acid solution will evaporate, but when the container is heated again and the solution is stirred, it will become liquid. For nitric acid that forms a hard shell and a thick layer, first break it up and then stir it into a paste. If necessary, add a few milliliters of water (see 6.1) to restore it to its normal state. 9.2 Test steps
Equilibrate the test container according to 9.1. In order to minimize the difference in equilibrium conditions, the clean sample should be placed in the container as quickly as possible. At the beginning of each test, a clean unplated copper or alloy sample should be placed in the container as an internal comparison sample to indicate that the test system is in operation. This steel sample should begin to turn black within a few hours. a) During the first 1 to 2 hours of the test, remove the stopper with a vent on the container and leave the cover pin slightly open to prevent leakage during the temperature increase of the system. When the test temperature is reached and the relative humidity is within the range of 85% to 90% (may take 1 to 2 hours), re-tighten the plug with the vent. b) Check the temperature and humidity in the container at appropriate time intervals within the first 2 to 3 hours of the specimen exposure and record them to ensure the consistency of the test conditions. This should be done before the end of the test. c) Continuous test for the specified time (when the test encounters a weekend),
d) After the test,Take out
generally 24 h test time can also be specified separately, the test system in the night (or three days cycle) before the test to cool the sample to room temperature. Re-container
) can be omitted.
is the step Na, the actual temperature and gradual monitoring of the container is still required routinely, it may be necessary to temporarily stir the container to confirm the acid drop test. Perform a new test
10 inspection and
of the sample using a light source (see 7.8 in the X10 microscope test county city
selection
a) if there is a mark (black discoloration) far away, the number of particles is in this position to show the adjustment, the shape of the bottom of the hole by the end of the movement and make the extension of the test period longer than
b) to count
, the following tips will help count: ||tt 1) Only count the discoloration of the skin products. 2) The smell of the product is not easy to remove by gentle blowing. When the sample is pushed, it changes. 3) When the sample is under light, if at least four of the spots are corrosion products originating from the measurement area, the sample is tested. After the test, the product is completely covered with silver or black spots. The bright gold cover is the urban area of Qingjing District, then the discoloration or stain is measured and counted. The discoloration in the measurement area should not be placed. The diameter of the corrosion products should be defined as: The number, size and position of the corrosion products with a true diameter less than 0.0 mm should not be counted. The microscopic scale should be determined by the person skilled in the art. Note that the micropores are as follows: ① diameter equal to or less than 12 mm ② diameter between 0.12 and 0.12 mm ③ diameter greater than 0.4 mm The number, size and position of the acceptable discoloration film or corrosion marks should be specified in the corresponding drawings or technical specifications. TYKoNKAa
A1 Quality of overlay
GB/T181792000
Appendix A
(Indicative Appendix)
Significance and Application
This test method is mainly used to determine the quality of overlay. In view of the fact that the overlay described in Chapter 1 of this standard is a protective layer, the porosity test reveals the complete degree of protection or coverage provided by the overlay, and its test results are also a measure of the control of the deposition process of the overlay. A2 Application to the quality of base coating
The special purpose of the wet sulfur test is to determine the quality of the base coating of silver alloy in the finishing system, which has a thin (1-2 βm or more) gold barrier layer on the base layer, because the pores of the key layer usually extend to this layer. ^3 Applied to test indoor environmental discoloration film
The humidity test is often used as an environmental test to simulate many indoor humid atmosphere discoloration films and discoloration dynamic effects. However, the discoloration film produced by this environmental test may not be similar in composition and chemical properties to the discoloration film produced in other service environments. Therefore, such product performance evaluation can only be combined with other performance test evaluations according to the provisions in the product manual. Relationship between AA and aging testwww.bzxz.net
Since corrosion and aging tests are used to determine the chemical stability of the transfer layer, the porosity test is different from them. However, in a good porosity test process, the corrosive agent should not invade the cover layer, but must purify, depolarize and/or activate the exposed metal from the pores, and sufficiently slow down the corrosion, so that the reaction products fill the pores and appear on the surface of the cover layer. A5 Sensitivity
Wet sulfur test is very sensitive, and it is an instinctive test for all pores in copper alloys. Nickel will not be corroded by wet sulfur vapor at a temperature below or equal to 10°C. Therefore, when the micropores or cracks do not penetrate the bottom layer to the base body, this test cannot be used to detect the micropores or cracks in the surface layer.
A6 Allowable porosity
The allowable porosity limit of the cover layer depends on the severity of the environment that the product may be exposed to during use or storage. At the same time, the location of the micropores on the surface is also important. If the number of micropores is small or far away from the main surface, they are often allowed to exist. A7 Geometric shape and selectivity considerations
This test can be used for test groups of various geometric shapes, such as curved surfaces. If there is room for discoloration in the exposed copper alloy area, this test can also be used for the short-term layer of the selected area. A8 Destructive test
This test is based on destructive testing. It reveals the presence of pores by discoloration film contamination test surface. Any workpiece that has passed this test should not be used again.
A9 Acceptance
The relationship between the porosity revealed by this method and the performance and service life of the product must be determined by the user of the test through actual experience or judgment. Therefore, some beryllium coatings may require no pores in the cover layer, while other coatings may allow a few pores on the main surface.
Appendix B
(Informed appendix)
References
Cl CLARKE. tars &. Interconnec.tion Technology Sympasium,Philadelphia,PA,October,1987,P. 47.TTIKAONIKaSince the pores of the key layer usually extend to this layer. ^3 Applied to the inspection of indoor environmental color-changing films
The humidity test is often used as an environmental test to simulate many indoor humid atmosphere color-changing films and color-changing effects. However, the color-changing films produced by this environmental test may not be similar in composition and chemical properties to those produced in other service environments. Therefore, such product performance evaluation can only be combined with other performance test evaluations according to the provisions in the product manual. Relationship between AA and aging test
Since corrosion and aging tests are used to determine the chemical stability of the transfer layer, the porosity test is different from them. However, in a good porosity test process, the corrosive agent should not invade the cover layer, but must purify, depolarize and/or activate the exposed metal from the pores, and sufficiently slow down the corrosion, so that the reaction products fill the pores and appear on the surface of the cover layer. A5 Sensitivity
Wet sulfur test is very sensitive, and it is an instinctive test for all pores in copper alloys. Nickel will not be corroded by wet sulfur vapor at a temperature below or equal to 10°C. Therefore, when the micropores or cracks do not penetrate the bottom layer to the base body, this test cannot be used to detect the micropores or cracks in the surface layer.
A6 Allowable porosity
The allowable porosity limit of the cover layer depends on the severity of the environment that the product may be exposed to during use or storage. At the same time, the location of the micropores on the surface is also important. If the number of micropores is small or far away from the main surface, they are often allowed to exist. A7 Geometric shape and selectivity considerations
This test can be used for test groups of various geometric shapes, such as curved surfaces. If there is room for discoloration in the exposed copper alloy area, this test can also be used for the short-term layer of the selected area. A8 Destructive test
This test is based on destructive testing. It reveals the presence of pores by discoloration film contamination test surface. Any workpiece that has passed this test should not be used again.
A9 Acceptance
The relationship between the porosity revealed by this method and the performance and service life of the product must be determined by the user of the test through actual experience or judgment. Therefore, some beryllium coatings may require no pores in the cover layer, while other coatings may allow a few pores on the main surface.
Appendix B
(Informed appendix)
References
Cl CLARKE. tars &. Interconnec.tion Technology Sympasium,Philadelphia,PA,October,1987,P. 47.TTIKAONIKaSince the pores of the key layer usually extend to this layer. ^3 Applied to the inspection of indoor environmental color-changing films
The humidity test is often used as an environmental test to simulate many indoor humid atmosphere color-changing films and color-changing effects. However, the color-changing films produced by this environmental test may not be similar in composition and chemical properties to those produced in other service environments. Therefore, such product performance evaluation can only be combined with other performance test evaluations according to the provisions in the product manual. Relationship between AA and aging test
Since corrosion and aging tests are used to determine the chemical stability of the transfer layer, the porosity test is different from them. However, in a good porosity test process, the corrosive agent should not invade the cover layer, but must purify, depolarize and/or activate the exposed metal from the pores, and sufficiently slow down the corrosion, so that the reaction products fill the pores and appear on the surface of the cover layer. A5 Sensitivity
Wet sulfur test is very sensitive, and it is an instinctive test for all pores in copper alloys. Nickel will not be corroded by wet sulfur vapor at a temperature below or equal to 10°C. Therefore, when the micropores or cracks do not penetrate the bottom layer to the base body, this test cannot be used to detect the micropores or cracks in the surface layer.
A6 Allowable porosity
The allowable porosity limit of the cover layer depends on the severity of the environment that the product may be exposed to during use or storage. At the same time, the location of the micropores on the surface is also important. If the number of micropores is small or far away from the main surface, they are often allowed to exist. A7 Geometric shape and selectivity considerations
This test can be used for test groups of various geometric shapes, such as curved surfaces. If there is room for discoloration in the exposed copper alloy area, this test can also be used for the short-term layer of the selected area. A8 Destructive test
This test is based on destructive testing. It reveals the presence of pores by discoloration film contamination test surface. Any workpiece that has passed this test should not be used again.
A9 Acceptance
The relationship between the porosity revealed by this method and the performance and service life of the product must be determined by the user of the test through actual experience or judgment. Therefore, some beryllium coatings may require no pores in the cover layer, while other coatings may allow a few pores on the main surface.
Appendix B
(Informed appendix)
References
Cl CLARKE. tars &. Interconnec.tion Technology Sympasium,Philadelphia,PA,October,1987,P. 47.TTIKAONIKa
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