CN104458548B - Method for detecting oxidation corrosion resistance of vacuum plating rose gold coating and plating layer - Google Patents
Method for detecting oxidation corrosion resistance of vacuum plating rose gold coating and plating layer Download PDFInfo
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- CN104458548B CN104458548B CN201410348820.XA CN201410348820A CN104458548B CN 104458548 B CN104458548 B CN 104458548B CN 201410348820 A CN201410348820 A CN 201410348820A CN 104458548 B CN104458548 B CN 104458548B
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Abstract
The invention discloses a method for detecting oxidation corrosion resistance of a vacuum plating rose gold coating and plating layer. The method comprises the following steps: (1) adding a suitable amount of dilute nitric acid solution with the mass percent of 8%-15% into a testing container; (2) suspending a specimen above the solution level of the dilute nitric acid solution in the testing container, and then sealing the opening of the testing container; (3) putting the sealed testing container into a closed container, adjusting the temperature of the closed container to be 35-40 DEG C, and keeping the temperature constant for 1-2 hours; and (4) after the step (3), taking out a specimen, washing clearly by water, and observing the coating of the specimen. The method for detecting the oxidation corrosion resistance of the vacuum plating rose gold coating and plating layer can be used for detecting the oxidation corrosion resistance of the vacuum plating rose gold coating and plating layer by utilizing the redox reaction of nitric acid (HNO3) and copper (Cu) in the vacuum plating rose gold coating and plating layer, and can detect the true oxidation corrosion resistance of the rose gold coating and plating layer in actual application rapidly, simply and conveniently.
Description
Technical field
The present invention relates to detection method, more particularly to a kind of Vacuum Deposition rose gold coated layer high oxidation and corrosion resistance detection
Method.
Background technology
In ornaments with billon series, rose gold (Rose Gold, abbreviation RG), because of the magnificent elegance of color and luster, becomes in fashion
In the outer clock and watch of Now Domestic, the trend fashion of jewelry industry.Electroplated rose golden cladding material is also liked by consumers in general.Pass
System water Gold-plating technique is gradually replaced because there is serious problem of environmental pollution by vacuum metallizing technology.Vacuum coating technology is not only
Environmental friendliness, and coating purity height, homogeneous thickness, the compactness and good with basal body binding force prepared using the technology.
The existing detection test to Vacuum Deposition rose gold coated layer corrosive nature mainly has neutral salt spray test and artificial perspiration
Two kinds of corrosion testing, the standard of execution is ISO-3160-2-2003 (E).And almost all of Vacuum Deposition rose gold coating now
The standard of neutral salt spray test (as shown in Figure 1) and artificial perspiration's corrosion testing that layer can pass through ISO-3160-2-2003 (E) will
Ask (as shown in Figure 2), but still deposited in actual applications by the Vacuum Deposition rose gold coated layer of two testing experiment standards
In serious oxide etch discoloration problem (as shown in Figure 3).Therefore, invention one kind can truly detect Vacuum Deposition rose gold coating
The detection method of layer high oxidation and corrosion resistance in actual applications just seems very urgent and necessary.
The content of the invention
For above-mentioned state of the art, the technical problem to be solved is, there is provided a kind of Vacuum Deposition Flos Rosae Rugosae
Golden coated layer high oxidation and corrosion resistance detection method, it can quickly, truly detect Vacuum Deposition rose gold coated layer in reality
Oxide etch performance in use, is that the progress of Vacuum Deposition rose gold Technology provides true and reliable test number with perfect
According to.
In order to solve above-mentioned technical problem, a kind of Vacuum Deposition rose gold coated layer antioxidant anticorrosive provided by the present invention
Energy detection method, the coated layer contains Au and Cu, and the detection method comprises the steps：
(1) dilute nitric acid solution that appropriate mass fraction is 8%～15% is added in test container；
(2) top of the dilute nitric acid solution liquid level for sample being hung in the test container, then by the survey
The opening sealing of examination container；
(3) by sealing after the test container be put in hermetic container, adjust hermetic container temperature be 35～40 DEG C,
Constant temperature 1～2 hour at this temperature；
(4) after step (3), sample is taken out, after being rinsed well with water, observes sample coating.
Wherein in one embodiment, in step (1), the volume of the dilute nitric acid solution in the test container is more than
100ml。
Wherein in one embodiment, in step (1), the test container is beaker.
The dilute nitric acid solution wherein in one embodiment, in step (2), in the sample and the test container
The distance of liquid level is more than 30mm.
Wherein in one embodiment, in step (2), the sample hangs on the test by rubber band and Glass rod
In container.
Wherein in one embodiment, in step (2), the opening of the test container is close by plastic sheeting and rubber band
Envelope.
Wherein in one embodiment, in step (3), constant temperature time is 2 hours.
Wherein in one embodiment, in step (3), the hermetic container is accurate baking oven.
Wherein in one embodiment, described Vacuum Deposition rose gold coated layer high oxidation and corrosion resistance detection method is also wrapped
The step of including the Lab values of sample before the determination test being arranged at before the step (2), it is arranged at after the step (4)
The step of after determination test the step of the Lab values of sample and according to forward and backward Lab values calculating value of chromatism is tested.
The Vacuum Deposition rose gold coated layer high oxidation and corrosion resistance detection method of the present invention, using nitric acid (HNO3) and vacuum
The redox reaction of copper (Cu), realizes the high oxidation and corrosion resistance to Vacuum Deposition rose gold coated layer in plating rose gold coated layer
Detection, the detection method can detect that rose gold coated layer real high oxidation and corrosion resistance in actual applications, and quickly,
It is easy.
Additional technical feature of the present invention has the advantage that will be said in this specification specific embodiment part
It is bright.
Description of the drawings
Fig. 1 is for Jing the conventional rose gold coated layer pattern of the Vacuum Deposition of (a) before 48h neutral salt spray tests, rear (b)；
Fig. 2 is for Jing the conventional rose gold coated layer pattern of the Vacuum Deposition of (a) before 48h artificial perspiration's corrosion testings, rear (b)；
Fig. 3 be it is actually used during because of the Vacuum Deposition routine rose gold coated layer pattern of oxidation stain；
Fig. 4 is coated layer pattern of the sample of the embodiment of the present invention one after antioxidant anticorrosive test；
Fig. 5 is coated layer pattern of the sample of the embodiment of the present invention two after antioxidant anticorrosive test.
Specific embodiment
Below with reference to the accompanying drawings and in conjunction with the embodiments the present invention is described in detail.It should be noted that not conflicting
In the case of, the feature in following embodiment and embodiment can be mutually combined.
Find that Vacuum Deposition rose gold coating laminate is (such as Vacuum Deposition rose gold coating through the present inventor's research
Wrist-watch adnexa, pieces of ornament accessories etc. of layer) coated layer mainly contain Au and Cu, the oxide etch performance of the coated layer mainly with painting
The content and Cu of Cu have with the homogeneity (i.e. with the Technology of Vacuum Deposition rose gold coated layer) of the phase melting range degree of Au in coating
Close, therefore the redox reaction of oxidant and copper (Cu) in Vacuum Deposition rose gold coated layer can be utilized, realize to Vacuum Deposition
The detection of rose gold coated layer high oxidation and corrosion resistance.However, the species of oxidant is more, contrast test effect, it is economical into
This and with reference to invention design principle on the premise of, have finally chosen with preferable oxidisability and volatile HNO3As this detection
The oxidant of method.
The Vacuum Deposition rose gold coated layer high oxidation and corrosion resistance detection method of the present invention is comprised the following steps that：
The dilute nitric acid solution that mass fraction is 8%～15%, test container is added to be preferably in step (1), test container
Beaker.If HNO3Solution concentration is too high, and highly volatile, acid mist is dense, and oxide etch is extremely strong, easily to testing equipment (precision high temperature
Baking oven) larger corrosion failure is caused, and using the HNO of high concentration3Carry out high oxidation and corrosion resistance test, the safety of test
Difference, is also easy to produce test incident；But, if HNO3Solution concentration is too low, and oxidisability is weaker, and test period is long, work efficiency
It is low.Through lot of experiments.Present invention determine that HNO3Solution concentration is 8%～15% (mass fraction), under this concentration conditions, HNO3
Solution oxide is moderate, and test period is 1-2h, in the moderate new 5N colors Flos Rosae Rugosae for keeping not oxidation stain in 1 year of actual wear
Golden coated layer can bear 2h Oxidation Resistance Tests, and wearing can not bear 2h antioxygens using the conventional rose gold coated layer of 2-3 month
Change test.
The top of step (2), the dilute nitric acid solution liquid level for sample being hung in the test container, then by institute
State the opening sealing of test container.Test finds, sample be immersed in dilute nitric acid solution will not oxide etch, therefore sample is hanged
The top of dilute nitric acid solution liquid level is hung over, using the dust technology and specimen reaction of volatilization, meanwhile, the opening of test container is sealed
Form the atmosphere of oxidisability.
Step (3), by sealing after the test container be put in hermetic container, adjust hermetic container temperature be 35～
40 DEG C, constant temperature 1～2 hour at this temperature.Because Vacuum Deposition rose gold coating product actual wear temperature be room temperature, the highest temperature
Not over 40 DEG C, in addition the temperature of artificial perspiration's corrosion testing is 40 DEG C to degree, and because the low test period of temperature is long, work is imitated
Rate is low, and temperature is too high, and experimental safe is bad, therefore the test temperature of detection method is defined as into 35～40 DEG C.
Jing is tested, and under the conditions of afore-mentioned test, through the test of oxide etch in 1 hour, is kept for 1 year not aoxidizing change actual wear is moderate
Color, and if constant temperature time was more than 2 hours, the sample of the overwhelming majority all can corrode, therefore, in order to consider to test effect, by perseverance
The warm time is defined as 1～2 hour.
After step (4), step (3), sample is taken out, after being rinsed well with water, observe sample coating.The effective coating of sample
Without bad phenomenon such as discoloration, foaming, peeling, peelings, then it is qualified to be considered as.
With reference to embodiment, the invention will be further described, it should be noted that embodiment is not constituted to this
The restriction of the claimed scope of invention.
Embodiment one
(1) sample
Sample in the present embodiment is to cover on Vacuum Deposition routine rose golden wrist-watch, and its Coating thickness degree is respectively
0.20 μm (usual thickness standard in industry) and 0.40 μm (highest thickness calibration in industry).
(2) test procedure
Step 1., the preparation of 8%～15% dilute nitric acid solution：The concentrated nitric acid of 15～20ml is measured with graduated cylinder or measuring cup
(mass fraction be 60%～69%) in a clean beaker (500ml) (should be previously added in beaker appropriate amount of deionized water or
Distilled water (50ml or so)), then deionized water or distilled water diluting are to beaker 100ml graduation marks, it is standby after ultrasonic 5min.
2., by sample rubber band and Glass rod step is hung in beaker, away from liquid level more than 30mm at, it is then thin with plastics
Film and rubber band seal in beaker mouth.
3., by the beaker after sealing step is put in accurate baking oven, adjusts oven temperature to 35 DEG C, constant temperature 2h；
Step 4., afterwards, takes out sample, and is rinsed with tap water.After rinsing well, observation sample coating has non-oxidation to take off
Skin and discoloration, then sample coating is wiped with handss, observe the change of sample coating.
(3) result of the test
It is enclosed within Jing after the test of 2h high oxidation and corrosion resistances, in the process rinsed with tap water on Vacuum Deposition routine rose gold
In, rose gold coated layer flaking, oxide etch is serious, and bottom class Flos Rosae Rugosae layer gold is also oxidized to dark yellow, is wiped with handss and is applied
After coating, coated layer further comes off (as shown in Figure 4), and the sample is unqualified.And the wrist-watch of the rose gold coated layer is adopted,
Oxide etch Coloring Time in actual wear use is 2～4 months (as shown in Figure 3), and its erosion profile and the antioxidation
Pattern after corrosion testing is basically identical, therefore testing result is consistent with practical situation.
Embodiment two
(1) sample
Sample is to cover on the new 5N rose goldens wrist-watch of Vacuum Deposition, and its Coating thickness degree is respectively 0.10 μm and 0.20
μm。
(2) test procedure
Step 1., the preparation of 8%～15% dilute nitric acid solution：The concentrated nitric acid of 15～20ml is measured with graduated cylinder or measuring cup
(mass fraction be 60%～69%) in a clean beaker (500ml) (should be previously added in beaker appropriate amount of deionized water or
Distilled water (50ml or so)), then deionized water or distilled water diluting are to beaker 100ml graduation marks, it is standby after ultrasonic 5min.
2., by sample rubber band and Glass rod step is hung in beaker, away from liquid level more than 30mm at, it is then thin with plastics
Film and rubber band seal in beaker mouth；
3., by the beaker after sealing step is put in accurate baking oven, adjusts oven temperature to 40 DEG C, constant temperature 2h；
Step 4., afterwards, takes out sample, and is rinsed with tap water.After rinsing well, observation sample coating has non-oxidation to take off
Skin and discoloration, then sample coating is wiped with handss, observe the change of sample coating.
(3) result of the test
It is enclosed within the new 5N rose golds of Vacuum Deposition Jing after the test of 2h high oxidation and corrosion resistances, comes off without discoloration and coated layer,
During being rinsed with tap water, rose gold coated layer Cheng Yiwu comes off, the situation of the effective coated layer No oxidation corrosion of sample
Occur, wiped after coated layer with handss, effective coated layer still occurs without the situation that coated layer comes off, and the sample is unqualified.Using
The wrist-watch of the rose gold coated layer, after actual wear is used 8 months, still occurs without obvious oxide etch discoloration,
Therefore testing result is consistent with practical situation.
Embodiment three
(1) sample
It is 0.20 that sample is Vacuum Deposition new 5N rose goldens stainless steel substrates (1.2mm × 25mm × 60mm) coated layer thickness
μm。
(2) test procedure
1., using CM-700d type spectrophotometric color measurement instruments (Japanese Konica Minolta) step determines Vacuum Deposition 5N rose golds and applies
The brightness value (L*) of coating color, green angle value (a*) and champac chromatic value (b*).
Step 2., the preparation of 8%～15% dilute nitric acid solution：The concentrated nitric acid of 15～20ml is measured with graduated cylinder or measuring cup
(mass fraction be 60%～69%) in a clean beaker (500ml) (should be previously added in beaker appropriate amount of deionized water or
Distilled water (50ml or so)), then deionized water or distilled water diluting are to beaker 100ml graduation marks, it is standby after ultrasonic 5min.
3., by sample rubber band and Glass rod step is hung in beaker, away from liquid level more than 30mm at, it is then thin with plastics
Film and rubber band seal in beaker mouth；
4., by the beaker after sealing step is put in accurate baking oven, adjusts oven temperature to 35～40 DEG C, constant temperature 2h；
Step 5., afterwards, takes out sample, and is rinsed with tap water.After rinsing well, observation sample coating has non-oxidation to take off
Skin and discoloration, then sample coating is wiped with handss, observe the change of sample coating.
6., using CM-700d type spectrophotometric color measurement instruments (Japanese Konica Minolta) step is determined Jing after 2h Oxidation Resistance Tests
The brightness value (L*) of Vacuum Deposition 5N rose gold coated layer colors, green angle value (a*) and champac chromatic value (b*), and with test
Front comparison.
(3) result of the test
1. the new 5N rose golds coated layer of Vacuum Deposition takes off Jing after the test of 2h high oxidation and corrosion resistances without discoloration and coated layer
Fall, during being rinsed with tap water, rose gold coated layer Cheng Yiwu comes off, the feelings of the effective coated layer No oxidation corrosion of sample
Condition occurs, and is wiped after coated layer with handss, and effective coated layer still occurs without the situation that coated layer comes off, and the sample is qualified.
2. as shown in table 1, the new 5N rose golds coated layer color of the Vacuum Deposition Jing after 2h Oxidation Resistance Tests is without significant change.
Its value of chromatismCalculate by formula (1).
As known from Table 1, L* before and after the test of the Vacuum Deposition new 5N rose golds coated layer color Jing 2h high oxidation and corrosion resistances,
The difference of a*, b* is respectively 0.16, -0.04 and -0.98, value of chromatismFor 0.98NBS (aberration unit).According to American National
The criterion of the Bureau of Standards, value of chromatism between 0.5～1.5NBS when, feel that aberration degree is slight, i.e. Jing 2h antioxidant anticorrosives
Rose gold coated layer is without obvious aberration before and after test.
The change of the new 5N rose golds coated layer color L*a*b* value of Vacuum Deposition before and after the test of the Jing 2h antioxidant anticorrosives of table 1
Situation
To sum up, by the Vacuum Deposition rose gold coated layer high oxidation and corrosion resistance detection method of the present invention, realize to true
The detection of the high oxidation and corrosion resistance of sky plating rose gold coated layer, the detection method can detect that rose gold coated layer actually should
The real high oxidation and corrosion resistance with, and quickly, it is easy.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more concrete and detailed, but and
Therefore the restriction to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, some deformations and improvement can also be made, these belong to the guarantor of the present invention
Shield scope.
Claims (9)
1. a kind of Vacuum Deposition rose gold coated layer high oxidation and corrosion resistance detection method, the coated layer contains Au and Cu, and it is special
Levy and be, the detection method comprises the steps：
(1) dilute nitric acid solution that appropriate mass fraction is 8%～15% is added in test container；
(2) top of the dilute nitric acid solution liquid level for sample being hung in the test container, then holds the test
The opening sealing of device；
(3) by sealing after the test container be put in hermetic container, adjust hermetic container temperature be 35～40 DEG C, here
At a temperature of constant temperature 1～2 hour；
(4) after step (3), sample is taken out, after being rinsed well with water, observes sample coating.
2. Vacuum Deposition rose gold coated layer high oxidation and corrosion resistance detection method according to claim 1, it is characterised in that
In step (1), the volume of the dilute nitric acid solution in the test container is more than 100ml.
3. Vacuum Deposition rose gold coated layer high oxidation and corrosion resistance detection method according to claim 1, it is characterised in that
In step (1), the test container is beaker.
4. Vacuum Deposition rose gold coated layer high oxidation and corrosion resistance detection method according to claim 1, it is characterised in that
In step (2), the distance of the dilute nitric acid solution liquid level in the sample and the test container is more than 30mm.
5. Vacuum Deposition rose gold coated layer high oxidation and corrosion resistance detection method according to claim 1, it is characterised in that
In step (2), the sample is hung in the test container by rubber band and Glass rod.
6. Vacuum Deposition rose gold coated layer high oxidation and corrosion resistance detection method according to claim 1, it is characterised in that
In step (2), the opening of the test container is sealed by plastic sheeting and rubber band.
7. Vacuum Deposition rose gold coated layer high oxidation and corrosion resistance detection method according to claim 1, it is characterised in that
In step (3), constant temperature time is 2 hours.
8. Vacuum Deposition rose gold coated layer high oxidation and corrosion resistance detection method according to claim 1, it is characterised in that
In step (3), the hermetic container is accurate baking oven.
9. Vacuum Deposition rose gold coated layer high oxidation and corrosion resistance detection side as claimed in any of claims 1 to 8
Method, it is characterised in that also including before the determination test being arranged at before the step (2) the step of the Lab values of sample, be arranged at
Aberration is calculated after determination test after the step (4) the step of the Lab values of sample and according to forward and backward Lab values are tested
The step of value.
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| CN106282959A (en) * | 2016-08-12 | 2017-01-04 | 创隆实业(深圳)有限公司 | A kind of rose gold aftertreatment technology |
| CN107014742A (en) * | 2017-04-14 | 2017-08-04 | 利郎(中国)有限公司 | A kind of decay resistance detection method of metal zip fastener |
| CN107621437B (en) * | 2017-09-07 | 2019-11-29 | 珠海罗西尼表业有限公司 | The detection method of the corrosion resistance of indicator |
| CN109668958A (en) * | 2018-12-10 | 2019-04-23 | 江苏天鹏电源有限公司 | Wall coating detection method in a kind of li battery shell |
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| CN201780254U (en) * | 2010-07-21 | 2011-03-30 | 上海梅山钢铁股份有限公司 | Sulfuric acid dew point corrosion resisting tester |
| CN102116730A (en) * | 2010-12-09 | 2011-07-06 | 中兴通讯股份有限公司 | Method for testing porosity of electric connector gold-plating layer |
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| CN103645187A (en) * | 2013-12-31 | 2014-03-19 | 广州天至环保科技有限公司 | Test reagent for realizing online rapid nondestructive test of quality of gold plating layer and using method of test reagent |
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| CN201780254U (en) * | 2010-07-21 | 2011-03-30 | 上海梅山钢铁股份有限公司 | Sulfuric acid dew point corrosion resisting tester |
| CN102116730A (en) * | 2010-12-09 | 2011-07-06 | 中兴通讯股份有限公司 | Method for testing porosity of electric connector gold-plating layer |
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