CN102116730B - Method for testing porosity of electric connector gold-plating layer - Google Patents
Method for testing porosity of electric connector gold-plating layer Download PDFInfo
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- CN102116730B CN102116730B CN 201010580698 CN201010580698A CN102116730B CN 102116730 B CN102116730 B CN 102116730B CN 201010580698 CN201010580698 CN 201010580698 CN 201010580698 A CN201010580698 A CN 201010580698A CN 102116730 B CN102116730 B CN 102116730B
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Abstract
The invention provides a method for testing the porosity of an electric connector gold-plating layer, which comprises the following steps of: (1) cleaning the surface of a sample; (2) hanging the sample in a sealed container; (3) preparing sodium hypochlorite solution and acid liquor, mixing the sodium hypochlorite solution with the acid liquor and pouring the mixture into the sealed container tobe sealed together with the sample, and standing still for 30 to 50 minutes, wherein the level of the mixed solution is lower than the sample and the temperature inside the sealed container is 21 to 25 DEG C; (4) drying the sample; and (5) observing the surface of the sample, calculating the number of corrosion spots according to the size of every observed corrosive, then adding up all the numbers of the corrosion spots in the test region, and calculating the porosity according to the total number of the corrosion spots and the test area of the sample. The method obtains the porosity simply, conveniently and accurately by mixing the hypochlorite solution with the acid liquor in the sealed container, performing chemical reaction between volatile gas and the sample and reasonably controlling time and space, the test process of the method is completed in the sealed container, and the test medium is nonhazardous and is extremely environmentally-friendly and safe.
Description
Technical field
The present invention relates to chemical technology field, relate in particular to a kind of method for testing porosity of electric connector gold-plating layer.
Background technology
At present as shown in Figure 1, most electric connector terminals are that aldary 1 is made, and common meeting corrosion in environment for use is such as oxidation, sulfuration etc.In order to prevent aldary 1 corrosion, keep the long-time stability on electric connector Metal Contact surface, often electroplate one deck noble metal-Jin and alloy 3 thereof at electric connector terminal.In addition, for prevent copper 1 with golden 3 mutually counterdiffusion and aldary 1 corrosion product diffuse to Gold plated Layer 3 surfaces, between copper 1 and Gold plated Layer 3, electroplate one deck nickel dam 2.
Because price of gold rises steadily, for reducing cost, Gold plated Layer 3 is thinned to below the 1 μ m gradually, so that Gold plated Layer 3 surfaces are prone to micropore.In the very thin coat of metal, the hole directly possibility by coating is very large, if base metal is exposed to corrosive atmosphere by these holes, hole corrosion will occur, especially under humid atmosphere, Gold plated Layer adsorption moisture, the water-soluble formation electrolytic solution of corrosive gas in the atmosphere or solubility dust, make generation primary element reaction between gold and the base material by micropore, the insulation erosion of generation spreads to surface in contact, finally causes resistance rising and loose contact between the contact.Therefore porosity becomes an important indicator estimating electric connector Gold plated Layer quality.
At present the detection method of Gold plated Layer surface porosity factor mainly is divided into four large classes: 1. gas exposes etch; 2. salt-fog test; 3. electrolysis visualization method; 4. paste filter paper method.
In standard GB/T17720-1999 (commentary of metal cladding ferroxyl test), ISO10308-2006 (Metallic coatings-Review of porosity tests), ASTM B765-2003 (Standardguide for selection of porosity and gross defect tests for electrodeposits andrelated metallic coatings) has done specified in more detail to the porosity method of inspection of nickel/gold in the copper substrate.
1. gaseous exposure method
The gas that uses in the method mainly contains SO
2, H
2S, H
2S/SO
2, H
2SO
3/ SO
2, HNO
3Steam etc.These methods have high requirements to experimental enviroment, test unit and test reagent, and gases used equal tool strong impulse and toxicity, can cause severe contamination to atmosphere, and also there is potential safety hazard in the test operation person.
2. salt-fog test
The method is mainly used certain density sodium chloride solution at a certain temperature, the long-time interior spraying that continues.This method is simple to operate, and shortcoming is to need special instruments, and is consuming time oversize, and non-test zone corrosion product easily spreads to test zone and causes porosity to be difficult for accurately calculating in test.At present most productions and use manufacturer estimate quality of coating qualitatively with the method.
3. electrolysis video picture method of testing
The method mainly contains the test of dimethylglyoxime paper Electrolysis, the test of cyclohexanedionedioxime paper Electrolysis.This method is simple to operate, and it is less that assay is affected by operating personnel.Shortcoming is to need special instrument, and its test paper and developer need special the making, and the detection operation that relates to gold plate on the nickel coating is poisonous operation, thereby substantially seldom has now producer to use.
4. paste filter paper method
The method mainly is to adopt CdS filter paper to be attached to specimen surface, calculates hole according to the spot on the filter paper.The method operation is comparatively simple, but employed CdS is hypertoxic, and there is potential safety hazard in experiment operator.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of method for testing porosity of electric connector gold-plating layer of simple, safe, convenient, accurate and environmental protection.
In order to address the above problem, the invention provides a kind of method for testing porosity of electric connector gold-plating layer, may further comprise the steps:
(1) cleaning sample surfaces;
(2) sample in the described step (1) is mounted in the closed container;
(3) liquor natrii hypochloritis of preparation 2-8wt% and the acid solution of 1-5wt%, and these two kinds of solution are mixed to pour in the described closed container left standstill 30-50 minute with the common sealing of sample, the mixed solution liquid level is lower than sample, and temperature is 21 degrees centigrade-25 degrees centigrade in the closed container;
(4) taking out sample from described closed container dries;
(5) observe sample surfaces after the oven dry, according to the observation to each erosion dimension conversion become the hot spot number, then add up all hot spot numbers of test zone, and calculate porosity according to total hot spot number and sample test area:
Porosity=total hot spot number/sample test area; Wherein, the unit of described porosity is/square centimeter.
Further, adopt the 5wt% liquor natrii hypochloritis of same ratio to mix with the acid solution of 2wt% in the described step (3).
Further, in the described step (5), erosion size and hot spot number conversion relation are as follows:
| The erosion size | Conversion hot spot number |
| Maximum outside diameter is below 0.05 millimeter | 0 |
| Maximum outside diameter is greater than 0.05 millimeter and below 0.5 |
1 |
| Maximum outside diameter is greater than 0.5 |
2 |
| The erosion area surpasses test zone area 50% | 20 |
Further, in the described step (4), this sample is put into 120-130 degree centigrade of baking oven baking dried at least ten minutes.
Further, the mixed solution liquid level is 2-3 centimetre apart from height of specimen in the described step (3).
Further, the support that adopts inert material to make in the described step (2) mounts sample.
Further, mixed liquor volume is the 20%-30% of described closed container volume in the described step (3).
The present invention has following advantage:
1, the present invention adopts and mix liquor natrii hypochloritis and acid solution in closed container; volatilization gas and sample carry out chemical reaction; and rationally control time, space; thereby simple, convenient and obtain exactly porosity; test process of the present invention is finished in closed container in addition; very environmental protection, and tested media nonhazardous, security is very high.
2, sample is 2-3 centimetre apart from liquid level among the present invention, liquor natrii hypochloritis and acid solution mixed solution account for the 20%-30% of closed container volume, time of repose is 30-50 minute, not only effectively utilizes tested media, and greatly improves testing efficiency and test accuracy.
Description of drawings
Below in conjunction with accompanying drawing embodiments of the present invention are described further:
Fig. 1 shows electric connector coating structure schematic diagram;
Fig. 2 shows test structure schematic diagram in a kind of method for testing porosity of electric connector gold-plating layer closed container of the present invention;
Fig. 3 shows the rear structural representation of a kind of method for testing porosity of electric connector gold-plating layer test of the present invention.
Embodiment
The present invention includes following steps:
(1) cleaning sample surfaces to sample surfaces totally without dirt.In this process, observe and the cleaning sample surfaces for convenient, usually need to adopt 20 power microscopes.In cleaning during sample surfaces, can adopt clean tweezers, lens wiping paper or cotton wipe samples surface or use and dry blow off behind the surperficial foul until sample surfaces is clean without the oil gas body.
(2) sample in the step (1) is mounted in the closed container.Sample is mounted in the closed container, can avoids sample test face to be stopped, affect test result.
(3) liquor natrii hypochloritis of preparation 5wt% and the acid solution of 2wt%, this acid solution can adopt hydrochloric acid, nitric acid or sulfuric acid solution.Test structure is poured these two kinds of solution in the closed container 9 into according to the same ratio mixing as shown in Figure 2, and this closed container 9 can adopt the tank body with hermetically-sealed construction, and sample 7 is mounted in this closed container 9 by support 8.Sample 7 rested on this closed container 9 interior 30-50 minutes with mixed solution 6 common sealings, and wherein: mixed solution 6 liquid levels are lower than sample 7, and closed container 9 interior temperature are 21 degrees centigrade-25 degrees centigrade.Under this condition, the volatilization gas that guarantees mixed solution 6 reactions fully and sample 7 surfaces react, reach the purpose of accurate test.
(4) taking out sample from closed container dries.The purpose of oven dry spreads fast for avoiding reacting erosion, affects test accuracy.
(5) sample surfaces after the observation oven dry is observed for convenient, usually adopts 20 power microscopes.It is red or green that erosion is generally, and red erosion is oxide, and green erosion is chloride.Under microscopic examination, measure the size of each erosion, and according to the observation to each erosion size be converted into the hot spot number:
| The erosion size | Conversion hot spot number |
| Maximum outside diameter is below 0.05 millimeter | 0 |
| Maximum outside diameter is greater than 0.05 millimeter and below 0.5 |
1 |
| Maximum outside diameter is greater than 0.5 |
2 |
| The erosion area surpasses test zone area 50% | 20 |
Add up all hot spot numbers of test zone, and calculate porosity according to total hot spot number and sample test area:
Porosity (individual/square centimeter)=total hot spot number/sample test area.
Among the present invention, in the step (4), this sample is put into 120-130 degree centigrade of baking oven baking dried at least ten minutes.For energy savings, reduction cost, usually take off limit value, namely toasted ten minutes.
Among the present invention, the mixed solution liquid level is 2-3 centimetre apart from height of specimen in the step (3).Improve response availability, and can corresponding reduction mixed solution concentration and capacity, so that test reaches ceiling effect.
Among the present invention, the support that adopts inert material to make in the step (2) mounts sample.Can adopt the materials such as glass and teflon.
Among the present invention, the mixed liquor volume of the acid solution of the liquor natrii hypochloritis of 5wt% and 2wt% is the 20%-30% of closed container volume in the step (3).
Reaction between mixed solution of the present invention and coating and porosity test philosophy are as follows:
(1) reaction mechanism
The reaction mechanism of measuring porosity is that hypochlorite generates hypochlorous acid with the acid combination, and the unstable horse back of hypochlorous acid decomposes generation HCl and O
2, HCl and O
2The nickel dam and the reaction of matrix copper that expose with the Gold plated Layer surface produce the green/red spot.As shown in Figure 3, electric connector comprises respectively metal level 1 (being copper), nickel coating 2 and Gold plated Layer 3, has hole on nickel coating 2 and the Gold plated Layer 3, so that the copper that comes out, nickel and HCl and O
2Reaction generates respectively chloride and the oxide 4 of chlorination of copper thing and oxide 5 and nickel, and demonstrates green and red.Its reaction mechanism is as follows:
ClO
-+H
+→HClO 2HClO→2HCl+O
2
Ni+2HCl→NiCl
2 2Ni+O
2→2NiO NiO+2HCl→NiCl
2
Cu+2HCl→CuCl
2 2Cu+O
2→2CuO CuO+2HCl→CuCl
2
(2) impact of the effect of each component of test solution and humiture and time
The effect of sodium hypochlorite: the principal ingredient of mixed solution provides chlorine and oxygen.
The effect of acid: provide hydrogen ion to be combined with the hypochlorite ion, discharge and detect gas HCl and O
2
Humiture: temperature is larger on the reaction rate impact, and excess Temperature is swift in response, and the reaction corrosion product can spread at the hole place and cause the corroded area erroneous judgement; Humidity effect HCl and O
2Diffusion, the excessive reaction of humidity is slowed down, and easily causes hole corrosion to spread.
Time: open-assembly time is larger on the hole impact, and the time, longer reaction corrosion product was more, and corrosion product spreads also more at the gold layer, cause interstitial surface area also larger.
Beneficial effect of the present invention:
1, the invention provides a kind of quick, simple and convenient, safe porosity of electric connector gold-plating layer method of inspection, satisfy the surface quality examination requirements that industrialization is produced.
2, the present invention is take common chlorinated lime as raw material, and the reagent price that conveniently is easy to get is comparatively cheap, and other adopts common exsiccator is checkout equipment, and the whole detection expense is cheap.
3, the Gold plated Layer of the applicable different-thickness of method provided by the invention test.
In sum; being preferred embodiment of the present invention only below, is not for restriction protection scope of the present invention, therefore; all any modifications of doing within the spirit and principles in the present invention, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. a method for testing porosity of electric connector gold-plating layer is characterized in that, may further comprise the steps:
(1) cleaning sample surfaces;
(2) sample in the described step (1) is mounted in the closed container;
(3) liquor natrii hypochloritis of preparation 2-8wt% and the acid solution of 1-5wt%, and these two kinds of solution are mixed to pour in the described closed container left standstill 30-50 minute with the common sealing of sample, the mixed solution liquid level is lower than sample, temperature is 21 degrees centigrade-25 degrees centigrade in the closed container, wherein hypochlorite and acid are in conjunction with generating hypochlorous acid, and the unstable horse back decomposition of hypochlorous acid generates HCl and O
2, HCl and O
2The nickel dam that exposes with the Gold plated Layer surface and the reaction of matrix copper produce the green/red spot, the volatilization gas that guarantees the mixed solution reaction fully and sample surfaces react;
(4) taking out sample from described closed container dries;
(5) observe sample surfaces after the oven dry, according to the observation to each erosion dimension conversion become the hot spot number, then add up all hot spot numbers of test zone, and calculate porosity according to total hot spot number and sample test area:
Porosity=total hot spot number/sample test area; Wherein, the unit of described porosity is/square centimeter.
2. method for testing porosity of electric connector gold-plating layer as claimed in claim 1 is characterized in that: adopt the 5wt% liquor natrii hypochloritis of same ratio to mix with the acid solution of 2wt% in the described step (3).
3. method for testing porosity of electric connector gold-plating layer as claimed in claim 1, it is characterized in that: in the described step (5), erosion size and hot spot number conversion relation are as follows:
4. method for testing porosity of electric connector gold-plating layer as claimed in claim 1 is characterized in that: in the described step (4), this sample is put into 120-130 degree centigrade of baking oven baking dried at least ten minutes.
5. method for testing porosity of electric connector gold-plating layer as claimed in claim 1 is characterized in that: the mixed solution liquid level is 2-3 centimetre apart from height of specimen in the described step (3).
6. method for testing porosity of electric connector gold-plating layer as claimed in claim 1 is characterized in that: adopt the support of inert material making to mount sample in the described step (2).
7. method for testing porosity of electric connector gold-plating layer as claimed in claim 1 is characterized in that: mixed liquor volume is the 20%-30% of described closed container volume in the described step (3).
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|---|---|---|---|
| CN 201010580698 CN102116730B (en) | 2010-12-09 | 2010-12-09 | Method for testing porosity of electric connector gold-plating layer |
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|---|---|---|---|
| CN 201010580698 CN102116730B (en) | 2010-12-09 | 2010-12-09 | Method for testing porosity of electric connector gold-plating layer |
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| CN102116730B true CN102116730B (en) | 2013-10-16 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102749424B (en) * | 2012-07-31 | 2016-06-22 | 竞陆电子(昆山)有限公司 | Dredge cell size gaseous test instrument |
| CN102914492A (en) * | 2012-10-18 | 2013-02-06 | 北京邮电大学 | Method for determining porosity of gold plating layer by utilizing sulfite solution |
| CN103163058A (en) * | 2013-03-25 | 2013-06-19 | 北京邮电大学 | Method for measuring porosity of nickel-base silver cladding by utilizing sulphurous acid steam |
| CN103308439B (en) * | 2013-06-18 | 2015-04-08 | 北京科技大学 | Method for evaluating effective porosity of metal corrosion product film |
| CN104458548B (en) * | 2014-07-21 | 2017-04-26 | 珠海罗西尼表业有限公司 | Method for detecting oxidation corrosion resistance of vacuum plating rose gold coating and plating layer |
| CN112649356B (en) * | 2020-11-29 | 2022-05-31 | 中国科学院金属研究所 | Method for evaluating material selection of abradable seal coating system from corrosion protection perspective |
| CN114112837B (en) * | 2021-11-12 | 2023-12-19 | 中航光电科技股份有限公司 | Method for detecting porosity of coating |
| CN114563322B (en) * | 2022-01-28 | 2023-12-19 | 武汉理工大学 | Characterization and regulation method for aluminum alloy surface corrosion microstructure in aluminum alloy/polymer laminated material |
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