CN102312232B - Environment-friendly copper and copper alloy surface passivation treatment fluid and passivation treatment method - Google Patents
Environment-friendly copper and copper alloy surface passivation treatment fluid and passivation treatment method Download PDFInfo
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- CN102312232B CN102312232B CN2011102120555A CN201110212055A CN102312232B CN 102312232 B CN102312232 B CN 102312232B CN 2011102120555 A CN2011102120555 A CN 2011102120555A CN 201110212055 A CN201110212055 A CN 201110212055A CN 102312232 B CN102312232 B CN 102312232B
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Abstract
The invention discloses an environment-friendly copper and copper alloy surface passivation treatment fluid and its passivation treatment method. Water or ethanol is used as a solvent of the passivation treatment fluid and its solute contains an N-C heterocycle compound; when the solvent is water, the solute also contains at least one component selected from a carboxylic acid compound and pyrophosphate; and when the solvent is ethanol, the solute also contains at least one component selected from a thio-alcohol compound, a carboxylic acid compound and pyrophosphate. In comparison with the prior art, by the principle of combining large molecular weight solute molecules and small molecular weight solute molecules together for self assembly on the surface of copper and copper alloy, the passivation treatment fluid provided by the invention has a much better passivation effect than a passivation treatment fluid, the solute of which is a single N-C heterocyclic compound, contains no substances of polluting the environment and influencing the health of human body, is convenient to use, requires low price, and has a good application prospect in the market.
Description
Technical field
The present invention relates to the metal material surface processing technology field, be specifically related to inactivating treatment liquid and the deactivating process for the treatment of thereof of a kind of environment-friendly type copper and copper alloy surface.
Background technology
China Copper and copper alloy amount of finish are annual 1000 ten thousand tons of left and right, and its every annual value of production is greater than 6,000 hundred million yuan.Generally, after machined copper and copper alloy workpiece, need to carry out Passivation Treatment to it, to improve its anti-variable color and corrosion resistance.At present, copper and copper alloy products passivation mainly adopt the treatment solutions such as chromic acid or its mixture to clean, but use these treatment solutions to carry out containing hexavalent chromium in waste water after Cleaning and Passivation is processed, serious environment pollution and affect the healthy of operator.Therefore, how eliminating the hexavalent chromium in waste water after passivation, is the key issue that copper and copper alloy surface treatment technology need to solve.
At present, the method for environment-friendly type copper and copper alloy surface passivation is also had report, for example application number be the patent of invention of CN86103910.6 to adopt benzotriazole and polyvinyl alcohol be passivator, but this patent has still been used a small amount of chromic acid; Application number is that the patent of invention of CN200810187682.6 adopts benzotriazole 5-8g/l, 1-phenyl-5 mercapto tetrazole 2-4g/l, tartrate (or citric acid) 14-18g/l, Sodium orthomolybdate (or sodium wolframate) 2-4g/l, the mixed solution of sodium lauryl sulphate 0.5-1g/l carries out passivation to brass, but this passivating solution complicated component, and expensive Sodium orthomolybdate or sodium wolframate have been used; Application number is that the patent of invention employing phytic acid of CN201010217372.1 is passivator, but need to carry out under certain impressed voltage; Application number is that the patent of invention of CN201010595972.1 adopts the mixed solutions such as phytic acid, hydrogen peroxide, boric acid, polyoxyethylene glycol to carry out passivation to brass, but the method is very complicated with sample ingredient, and in phytic acid (phytinic acid), phosphorus content is very high, can cause the chemical oxygen demand (COD) in waste water to increase.
Summary of the invention
Technical purpose of the present invention is for the above-mentioned state of the art, providing a kind of provides the inactivating treatment liquid of a kind of environment-friendly type copper and copper alloy surface and utilizes the deactivating process for the treatment of of this inactivating treatment liquid to copper and copper alloy surface, and this inactivating treatment liquid has the advantages such as the material, the passivation effect that do not contain contaminate environment and affect HUMAN HEALTH be good, easy to use, cheap.
The present invention realizes that the technical scheme that above-mentioned technical purpose adopts is: the inactivating treatment liquid of a kind of environment-friendly type copper and copper alloy surface, its solvent is water or ethanol, solute includes the N-C heterocyclic compound, it is characterized in that: when solvent is water, also include at least a in carboxylic acid compound and pyrophosphate salt in solute; When solvent is ethanol, also include at least a in sulfur alcohol compound and carboxylic acid compound in solute.
In technique scheme:
Described N-C heterocyclic compound is preferably at least a in benzotriazole and oxine;
Described sulfur alcohol compound is preferably at least a in 1.2-dithioglycol, propane thiol and Dodecyl Mercaptan;
Described carboxylic acid compound is preferably at least a in formic acid, acetic acid, oxalic acid, propionic acid, butyric acid, formate, acetate, oxalate, propionic salt and butyrates;
The pH value scope of described inactivating treatment liquid is preferably 2～7.
In described inactivating treatment liquid, when solvent was water, the concentration range of benzotriazole was preferably the saturation concentration of 1g/l to benzotriazole, more preferably 10g/l～19g/l; The concentration range of carboxylic acid compound is 1g/l～20g/l, more preferably 5g/l～15g/l; The concentration range of pyrophosphate salt is 1g/l～20g/l, more preferably 1g/l～5g/l.
In described inactivating treatment liquid, when solvent was ethanol, the concentration range of oxine was that 0.1g/l is to its saturation concentration, more preferably 1g/l～5g/l; The concentration of sulfur alcohol compound is 0.1g/l～1g/l, more preferably 0.5g/l～1g/l.
The method of using inactivating treatment liquid of the present invention to process copper and copper alloy surface specifically comprises the steps:
The configuration of step 1, inactivating treatment liquid:
The solute that will include the N-C heterocyclic compound is soluble in water, then adds carboxylic acid compound and/or pyrophosphate salt, obtains inactivating treatment liquid; Perhaps,
The solute that will include the N-C heterocyclic compound is dissolved in alcohol solvent, then adds sulfur alcohol compound and/or carboxylic acid compound, obtains inactivating treatment liquid;
The surface degreasing of step 2, copper and copper alloy:
Be 5%～20% NaOH solution at mass percent concentration, perhaps in being 5%～20% KOH solution, mass percent concentration adds appropriate sodium lauryl sulphate, obtain mixing solutions, copper or copper alloy are put into this mixing solutions, are to clean 3 minutes～10 minutes under 40 ℃～70 ℃ at cleaning temperature;
Wherein, the concentration of sodium lauryl sulphate in mixing solutions is preferably 0.5g/l～10g/l, more preferably 2g/l; Cleaning temperature is preferably 60 ℃～70 ℃;
The surperficial oxide film dissolving of step 3, copper and copper alloy is processed:
Utilize mechanical polishing, chemical rightenning or number of patent application, for the method described in CN201110108791.6, copper or copper alloy are carried out the surface film oxide Transformatin;
Wherein, number of patent application is in CN201110108791.6, and the treatment process of removing copper and copper alloy surface oxide film with the treatment solution reduction specifically comprises the steps:
(1) configuration for the treatment of solution: reductive agent is added to the water the formation treatment solution, described reductive agent is one or more the mixture in xitix, hypophosphite, glucose, hydrazine and derivative thereof, azanol and derivative thereof, and the pH value of regulating treatment solution is 2～13;
(2) surface reduction of copper and copper alloy is processed: the treatment solution temperature is normal temperature to 90 ℃, and the copper after step 2 oil removing and copper alloy are immersed in treatment solution, takes out after surface reduction is copper and copper alloy true qualities, then cleaning, drying.
Hydrazine and derivative thereof described in above-mentioned (1) include but not limited to NH
2-NH
2, NH
2-NH
2H
2O, phenylhydrazine, R
1R
2N-NR
1R
2(R representation hydrocarbyl); Described azanol and derivative thereof include but not limited to N, N-diethyl hydroxylamine, N, N-dimethyl hydroxylamine, phosphatic hydroxylamine, Acetohydroxamic Acid, oxammonium sulfate, hydroxylamine chloride.
Step 4, copper and copper alloy surface Passivation Treatment:
The inactivating treatment liquid that copper after step 3 is processed or copper alloy are put into step 1 preparation carries out surface passivating treatment.
The inactivating treatment liquid of environment-friendly type copper provided by the invention and copper alloy surface is a kind of aqueous solution or ethanolic soln, wherein solute energy and copper and copper alloy generation self-assembling reaction, in the characteristic of copper and the densification of copper alloy surface self-assembly one deck, thereby realization is to the passivation effect of copper and copper alloy surface.Innovation of the present invention is, this solute not only includes the N-C heterogeneous ring compound, also includes at least a in carboxylic acid compound, sulfur alcohol compound and pyrophosphate salt.Because the molecular size range of each solute is different, its ability of self-assembly at copper and copper alloy surface is different, and the compactness extent of formed self assembled monolayer film is also different, thereby acts synergistically, and has improved on the whole the passivation effect of copper and copper alloy surface.especially when the molecular weight of each solute in inactivating treatment liquid differs larger, the larger solute of molecular weight is in copper and the larger characteristic of copper alloy surface self-assembly one deck molecular weight, this characteristic is because molecular chain is longer, some little spaces are arranged between molecule and molecule unavoidably, and the solute of molecular weight can be assembled among these spaces, to fill up these little spaces, thereby the characteristic in copper and the densification of copper alloy surface formation one deck, make copper and copper alloy and outside air and water isolated, copper and copper alloy surface passivation have been improved, erosion-resisting effect.
Color has considerable change when copper generation oxidation, and brass is dimmed, the red copper blackening.Experimental results show that:
Existing, brass after overpickling and polished finish two weeks left and right gloss in malaria can disappear, and three days color relations of red copper can change, especially larger in humidity, under the higher environment of temperature, its color disintegration rate is faster, for example in humidity, is 80%, temperature is under the condition of 70 ℃～90 ℃, the brass color and luster hold-time, the red copper color and luster hold-time was less than 2 hours less than 5 hours;
Existing, after overpickling and polished finish, the brass that the inactivating treatment liquid that is single N-C heterogeneous ring compound through solute is again processed in malaria through about 1 month gloss can disappear, and red copper can change through all color relations, and is especially larger in humidity, under the higher environment of temperature, its color disintegration rate is faster, for example in humidity, be 80%, temperature is that under the condition of 70 ℃～90 ℃, the brass color and luster hold-time, the red copper color and luster hold-time was less than 5 hours less than 50 hours;
But, in the present invention, after overpickling and polished finish, then copper and copper alloy after inactivating treatment liquid of the present invention is processed, have following effect:
(1) in malaria, brass nondiscoloration half a year, red copper nondiscoloration in three months;
(2) be 80% in humidity, temperature is under the condition of 70 ℃～90 ℃: the brass color and luster can keep more than 100 hours, and the red copper color and luster can keep more than 50 hours.
Therefore, compared with prior art, the inactivating treatment liquid of copper provided by the invention and copper alloy surface adopts the macromolecule solute molecule in conjunction with the principle of the common self-assembly of small molecular weight solute molecule at copper and copper alloy surface, has following advantage:
(1) passivation effect is far superior to the inactivating treatment liquid that solute is single N-C heterogeneous ring compound;
(2) not containing contaminate environment and affect the material of HUMAN HEALTH, is a kind of inactivating treatment liquid of environment-friendly type, produces a large amount of sexavalent chromes while having avoided Passivation Treatment and the problems such as contaminate environment and person health;
(3) easy to use, do not need after passivation to clean, but directly dry water saving;
(4) cheap, consumption is few and effective;
(5) applied widely, not only can carry out Passivation Treatment to copper alloy, and red copper (fine copper) is also had good passivation.
Therefore, copper provided by the invention and copper alloy surface inactivating treatment liquid and deactivating process for the treatment of thereof, have the advantages such as cost is low, easy to use, processing is rapid, effect is remarkable, environment protection health, has good market application foreground.
Embodiment
Below by specific embodiment, the present invention is described in further detail, it is pointed out that the following stated embodiment is intended to be convenient to the understanding of the present invention, and it does not played any restriction effect.
Following Passivation Treatment sample is the assembling red copper and cuts the copper alloy spray gun of chewing and assemble brass and cut the brass spray gun of chewing.
Comparing embodiment 1:
In order with following embodiment 1, to compare, in this comparative example, the Passivation Treatment sample is only carried out surface cleaning and the processing of deoxidation film, do not use passivating solution to carry out Passivation Treatment.Concrete steps are:
(1) adding the 2g/l sodium lauryl sulphate in mass percent concentration is 5%～20% NaOH solution, obtain mixing solutions, the Passivation Treatment sample is put into this mixing solutions, is to clean 5 minutes under 60 ℃ at cleaning temperature;
(2) utilize the Passivation Treatment sample after mechanical polishing is processed step (2) to carry out the surface film oxide Transformatin.
The comparative example 2:
In order further with following embodiment 1, to compare, in this comparative example, the Passivation Treatment liquid formula is: solvent is water, and solute is benzotriazole, and the mass concentration of benzotriazole is 10g/l.
Use above-mentioned inactivating treatment liquid to the concrete steps that the Passivation Treatment sample surfaces carries out Passivation Treatment to be:
(1) appropriate benzotriazole is water-soluble, making the mass concentration of benzotriazole is 10g/l, obtains inactivating treatment liquid;
(2) adding the 2g/l sodium lauryl sulphate in mass percent concentration is 5%～20% NaOH solution, obtain mixing solutions, the Passivation Treatment sample is put into this mixing solutions, is to clean 5 minutes under 60 ℃ at cleaning temperature;
(3) utilize the Passivation Treatment sample after mechanical polishing is processed step (2) to carry out the surface film oxide Transformatin;
(4) the Passivation Treatment sample after step (3) is processed is dipped in the inactivating treatment liquid of step 1 preparation and carries out Passivation Treatment, and keeping the Passivation Treatment liquid temp is 60 ℃, and soak time is 5 minutes, after processing 60 ℃ of oven dry 5 minutes.
Embodiment 1:
In the present embodiment:
The Passivation Treatment liquid formula is: solvent is water, and solute is benzotriazole and propionic acid, and wherein, the mass concentration of benzotriazole is 10g/l, and the mass concentration of propionic acid is 10g/l.
Use above-mentioned inactivating treatment liquid to the concrete steps that the Passivation Treatment sample surfaces carries out Passivation Treatment to be:
(1) appropriate benzotriazole is soluble in water, then add appropriate propionic acid, the mass concentration that makes benzotriazole is 10g/l, the mass concentration of propionic acid is 10g/l, makes and obtains inactivating treatment liquid;
(2) adding the 2g/l sodium lauryl sulphate in mass percent concentration is 5%～20% NaOH solution, obtain mixing solutions, the Passivation Treatment sample is put into this mixing solutions, is to clean 5 minutes under 60 ℃ at cleaning temperature;
(3) utilize the Passivation Treatment sample after mechanical polishing is processed step (2) to carry out the surface film oxide Transformatin;
(4) the Passivation Treatment sample after step (3) is processed is dipped in the inactivating treatment liquid of step 1 preparation and carries out Passivation Treatment, and keeping the Passivation Treatment liquid temp is 60 ℃, and soak time is 5 minutes, after processing 60 ℃ of oven dry 5 minutes.
Embodiment 2:
In the present embodiment:
The Passivation Treatment liquid formula is: solvent is ethanol, and solute is benzotriazole and Dodecyl Mercaptan, and wherein, the mass concentration of benzotriazole is 10g/l, and the mass concentration of Dodecyl Mercaptan is 1g/l.
Use above-mentioned inactivating treatment liquid to the concrete steps that the Passivation Treatment sample surfaces carries out Passivation Treatment to be:
(1) appropriate benzotriazole is dissolved in ethanol, then adds appropriate Dodecyl Mercaptan, the mass concentration that makes benzotriazole is 10g/l, and the mass concentration of Dodecyl Mercaptan is 1g/l, makes and obtains inactivating treatment liquid;
(2) adding the 2g/l sodium lauryl sulphate in mass percent concentration is 5%～20% NaOH solution, the Passivation Treatment sample is put into this mixing solutions, is to clean 10 minutes under 40 ℃ at cleaning temperature;
(3) utilize the Passivation Treatment sample after chemical rightenning is processed step (2) to carry out the surface film oxide Transformatin;
(4) the Passivation Treatment sample after step (3) is processed is dipped in the inactivating treatment liquid of step 1 preparation and carries out Passivation Treatment, and keeping the Passivation Treatment liquid temp is 60 ℃, and soak time is 5 minutes, after processing 60 ℃ of oven dry 5 minutes.
Example 3:
In the present embodiment:
The Passivation Treatment liquid formula is: solvent is water, and solute is benzotriazole and tetra-sodium, and wherein, the mass concentration of benzotriazole is 10g/l, and the mass concentration of tetra-sodium is 5g/l.
Use above-mentioned inactivating treatment liquid to the concrete steps that the Passivation Treatment sample surfaces carries out Passivation Treatment to be:
(1) appropriate benzotriazole is dissolved in ethanol, then adds appropriate tetra-sodium, the mass concentration that makes benzotriazole is 10g/l, and the mass concentration of tetra-sodium is 5g/l, makes and obtains inactivating treatment liquid;
(2) adding the 2g/l sodium lauryl sulphate in mass percent concentration is 5%～20% NaOH solution, obtain mixing solutions, the Passivation Treatment sample is put into this mixing solutions, is to clean 3 minutes under 70 ℃ at cleaning temperature;
(3) utilize number of patent application, for the method described in CN201110108791.6, the Passivation Treatment sample is carried out the surface film oxide Transformatin;
(4) the Passivation Treatment sample after step (3) is processed is dipped in the inactivating treatment liquid of step 1 preparation and carries out Passivation Treatment, and keeping the Passivation Treatment liquid temp is 60 ℃, and soak time is 5 minutes, after processing 60 ℃ of oven dry 5 minutes.
The comparative example 3:
In order with following examples 4, to compare, in this comparative example, the Passivation Treatment liquid formula is: solvent is ethanol, and solute is oxine, and the mass concentration of oxine is 2g/l.
Use above-mentioned inactivating treatment liquid to the concrete steps that the Passivation Treatment sample surfaces carries out Passivation Treatment to be:
(1) appropriate oxine is water-soluble, making the mass concentration of oxine is 2g/l, obtains inactivating treatment liquid;
(2) adding the 2g/l sodium lauryl sulphate in mass percent concentration is 5%～20% KOH solution, obtain mixing solutions, the Passivation Treatment sample is put into this mixing solutions, is to clean 5 minutes under 60 ℃ at cleaning temperature;
(3) utilize the Passivation Treatment sample after mechanical polishing is processed step (2) to carry out the surface film oxide Transformatin;
(4) the Passivation Treatment sample after step (3) is processed is dipped in the inactivating treatment liquid of step 1 preparation and carries out Passivation Treatment, and keeping the Passivation Treatment liquid temp is 60 ℃, and soak time is 5 minutes, after processing 60 ℃ of oven dry 5 minutes.
Embodiment 4:
In the present embodiment:
The Passivation Treatment liquid formula is: solvent is ethanol, and solute is oxine and propionic acid, and wherein, the mass concentration of oxine is 2g/l, and the mass concentration of propionic acid is 10g/l.
Use above-mentioned inactivating treatment liquid to the concrete steps that the Passivation Treatment sample surfaces carries out Passivation Treatment to be:
(1) appropriate oxine is soluble in water, then add appropriate propionic acid, the mass concentration that makes oxine is 2g/l, the mass concentration of propionic acid is 10g/l, makes and obtains inactivating treatment liquid;
(2) adding the 2g/l sodium lauryl sulphate in mass percent concentration is 5%～20% KOH solution, obtain mixing solutions, the Passivation Treatment sample is put into this mixing solutions, is to clean 5 minutes under 60 ℃ at cleaning temperature;
(3) utilize the Passivation Treatment sample after mechanical polishing is processed step (2) to carry out the surface film oxide Transformatin;
(4) the Passivation Treatment sample after step (3) is processed is dipped in the inactivating treatment liquid of step 1 preparation and carries out Passivation Treatment, and keeping the Passivation Treatment liquid temp is 60 ℃, and soak time is 5 minutes, after processing 60 ℃ of oven dry 5 minutes.
Embodiment 5:
In the present embodiment:
The Passivation Treatment liquid formula is: solvent is ethanol, and solute is oxine and Dodecyl Mercaptan, and wherein, the mass concentration of oxine is 2g/l, and the mass concentration of Dodecyl Mercaptan is 1g/l.
Use above-mentioned inactivating treatment liquid to the concrete steps that the Passivation Treatment sample surfaces carries out Passivation Treatment to be:
(1) appropriate oxine is soluble in water, then add appropriate Dodecyl Mercaptan, the mass concentration that makes oxine is 2g/l, the mass concentration of Dodecyl Mercaptan is 10g/l, makes and obtains inactivating treatment liquid;
(2) adding the 2g/l sodium lauryl sulphate in mass percent concentration is 5%～20% KOH solution, obtain mixing solutions, the Passivation Treatment sample is put into this mixing solutions, is to clean 5 minutes under 60 ℃ at cleaning temperature;
(3) utilize the Passivation Treatment sample after mechanical polishing is processed step (2) to carry out the surface film oxide Transformatin;
(4) the Passivation Treatment sample after step (3) is processed is dipped in the inactivating treatment liquid of step 1 preparation and carries out Passivation Treatment, and keeping the Passivation Treatment liquid temp is 60 ℃, and soak time is 5 minutes, after processing 60 ℃ of oven dry 5 minutes.
With the Passivation Treatment sample after processing in the various embodiments described above be 80% in humidity, temperature is to test under the condition of 90 ℃, obtains result shown in following table:
Sample after Passivation Treatment in above each embodiment is 80% in humidity, temperature is the interior baking of the baking oven of 70 ℃, observe the Passivation Treatment sample, namely assemble red copper and cut the copper alloy spray gun chewed and assembling brass and cut the brass spray gun of chewing and start to occur the needed time of variable color, the result that obtains is as shown in the table.
Above-described embodiment has been described in detail technical scheme of the present invention and beneficial effect; be understood that and the foregoing is only specific embodiments of the invention; be not limited to the present invention; all any modifications of making in principle scope of the present invention and improvement etc., within all should being included in protection scope of the present invention.
Claims (5)
1. the inactivating treatment liquid of environment-friendly type copper and copper alloy surface, its solvent is ethanol, solute includes the N-C heterocyclic compound, it is characterized in that: also include sulfur alcohol compound in solute; Described N-C heterocyclic compound is oxine, in described inactivating treatment liquid, the concentration range of oxine be 0.1g/l to its saturation concentration, the concentration of sulfur alcohol compound is 0.1g/l～1g/l.
2. the inactivating treatment liquid of environment-friendly type copper according to claim 1 and copper alloy surface is characterized in that: described sulfur alcohol compound is at least a in 1.2-dithioglycol, propane thiol and Dodecyl Mercaptan.
3. the inactivating treatment liquid of environment-friendly type copper according to claim 1 and copper alloy surface, it is characterized in that: the pH value scope of described inactivating treatment liquid is 2～7.
4. the inactivating treatment liquid of environment-friendly type copper according to claim 1 and copper alloy surface, it is characterized in that: in described inactivating treatment liquid, the concentration range of oxine is 1g/l～5g/l, and the concentration of sulfur alcohol compound is 0.5g/l～1g/l.
5. the method for the described inactivating treatment liquid processing copper of arbitrary claim and copper alloy surface in right to use requirement 1 to 4, is characterized in that: comprise the steps:
The configuration of step 1, inactivating treatment liquid:
The solute that will include the N-C heterocyclic compound is dissolved in alcohol solvent, then adds sulfur alcohol compound, obtains inactivating treatment liquid;
The surface degreasing of step 2, copper and copper alloy:
Be 5%～20% NaOH solution at mass percent concentration, perhaps in being 5%～20% KOH solution, mass percent concentration adds appropriate sodium lauryl sulphate, obtain mixing solutions, copper or copper alloy are put into this mixing solutions, are to clean 3 minutes～10 minutes under 40 ℃～70 ℃ in temperature;
The surperficial oxide film dissolving of step 3, copper and copper alloy is processed:
Utilize mechanical polishing or chemical rightenning to carry out the oxide film dissolving processing to copper and copper alloy;
Step 4, copper and copper alloy surface Passivation Treatment:
The inactivating treatment liquid that copper after step 3 is processed or copper alloy are put into step 1 preparation carries out surface passivating treatment.
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| CN2011102120555A CN102312232B (en) | 2011-07-27 | 2011-07-27 | Environment-friendly copper and copper alloy surface passivation treatment fluid and passivation treatment method |
| CN201310534594.XA CN103556142B (en) | 2011-07-27 | 2011-07-27 | The inactivating treatment liquid of environment-friendly type copper and copper alloy surface and deactivating process for the treatment of thereof |
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| CN103556142A (en) | 2014-02-05 |
| CN102312232A (en) | 2012-01-11 |
| CN103556142B (en) | 2016-05-11 |
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