CN101463462B - Invisible fastness anti-tarnishing layer for silver coin surface and preparation method - Google Patents
Invisible fastness anti-tarnishing layer for silver coin surface and preparation method Download PDFInfo
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- CN101463462B CN101463462B CN2007101590646A CN200710159064A CN101463462B CN 101463462 B CN101463462 B CN 101463462B CN 2007101590646 A CN2007101590646 A CN 2007101590646A CN 200710159064 A CN200710159064 A CN 200710159064A CN 101463462 B CN101463462 B CN 101463462B
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Abstract
The invention relates to a silver coin surface invisible tarnish resisting protective layer and a preparing method thereof, and solves the problem that the surfaces of silver coins are discolored after being placed for a long time. The preparing method is realized by the steps: (1) pretreatment of the silver coins; (2) vacuum-pumping; (3) aluminum target cleaning; (4) preparing an aluminum oxide protective layer by reaction magnetron sputtering; (5) aluminum target post treatment. The invisible aluminum oxide protective layer prepared by the invention has good tarnish resisting effect, protects the appearance quality of the silver coins and is long in guard time.
Description
Technical field
The present invention relates to protective layer and preparation method that a kind of silver coin surface forms, relate in particular to a kind of invisible fastness anti-tarnishing layer for silver coin surface and preparation method, belong to silver coin anti-discolouring technology.
Background technology
When silver and silver alloys use in atmospheric environment, because atomospheric corrosion can produce dark-coloured coherent film on its surface.So-called atomospheric corrosion is because the phenomenon that the thin layer corrodibility electrolytic solution that metal material surface adheres to causes.This electrolytic solution is mainly by the H of the relative humidity of air and the ppb level that contains
2S, NO
2, HCl, SO
2, O
3, Cl
2, ammonia and other organic gass form.Usually the variable color of metal under the natural atmosphere condition is because the etch of above-mentioned medium causes.
The variable color of silver and silver alloys has had a strong impact on silverware use, circulation, collection.This phenomenon not only exists in China, and other countries also face same puzzlement.The silver commemorative coin is as being the valuable artwork of purpose to view and admire and to collect, and the outward appearance and the color and luster on surface have great effect to its value.No matter all face at present the discoloration problem of silver coin in China or the mint of world other countries.
Mint, countries in the world and silverware manufacturer are studied for the anti-tarnishing ability that improves silverware, have now obtained remarkable progress, but still do not solve fully so far.Therefore, the reason and the mechanism of research silver coin generation variable color, corresponding safeguard procedures not only help the Development and Production of new silver coin, and for existing ancient times silver coin preservation, exhibition be significant.
Silver coin is generally made with fine silver, even handle meticulously, leaves in the environment of sealing, still can produce sulfide or other corrosion product after several days.Because silver coin surface exposed environments condition difference, corrosion product also has different.The above analysis result and document by its surface corrosion product color and luster difference, can divide and conclude following three kinds.
(1) Bao filbert rust staining layer does not influence the gloss on silver coin surface.The general casting time is not long, or the preservation environment preferably silver coin mostly be this kind state.
(2) rusty scale is thicker, and color obviously is different from matrix, has a strong impact on the gloss on silver coin surface.This type of corrosion mostly occurs in moist and environment that suspended particle is more.
(3) the long hickie of silver coin is examined under a microscope the crystal grain into white.
The silver coin brownish corrosion in surface mainly is a silver sulfide, also has tungsten sulfide, muriate, oxide compound, carbide, carbon monoxide, carbonate and carbonic acyl radical compound etc. to adhere to sometimes.Usually by effective constituent generation vulcanization reaction in silver and ambient air or the sweat, generate silver sulfide.Simultaneously, the deposited particles in the environment can cause generating the compound of sodium, potassium, silicon etc. in corrosion layer.In addition, produce these compounds after, the surface forms a plurality of small electrochemical primary cells, the silver coin variable color is even more serious.
The reason of silver coin generation hickie is more.The defective of material itself (as metal inclusion etc.), reasons such as the existence of corrosive medium and atmospheric moisture, electromagnetic radiation have caused silver coin surface passivation film destroy in the wrapping material degradation production of silver coin, production technique, water quality, the air, form activation/passivation corrosion cell, produced the corrosion product of chloride and sodium element, make the silver coin surface lose original gloss, macroscopic hickie occurred.
The silverware of the prior art especially anti-discolouring protective layer on silver coin surface changes the metal-like of silver coin easily and has visibility, therefore causes the undesirable and guard time weak point of silver coin visual appearance.
Summary of the invention
The present invention is directed to above-mentioned problems of the prior art; carry out a large amount of groping and Test Summary; developed a kind of invisible fastness anti-tarnishing layer for silver coin surface; solved that anti-discolouring protective layer of the prior art changes the metal-like of silver coin or be not invisible fully; cause the problem that the silver coin visual appearance is undesirable and guard time is short; and the present invention operation is simple, reduced production cost.
Another object of the present invention has been to provide a kind of preparation method of invisible fastness anti-tarnishing layer for silver coin surface.
Technical scheme of the present invention is as follows:
The outside surface of silver coin is provided with protective layer of alumina.
Preparation method of the present invention comprises the steps:
The cleaning of silver coin: at ambient temperature, with silver coin ultrasonic cleaning 1-3 time in dehydrated alcohol, each 2-10min, clean for the second time finish after with the silver coin hot blast drying;
Vacuumize: silver coin is put into vacuum chamber, and back of the body end vacuum is taken out and is caused 0.005Pa;
The cleaning of aluminium target: feeding purity to vacuum chamber is 99.99% high-purity Ar gas, make air pressure between 0.2-0.5Pa, on magnetron sputtering target, apply a 300-1000 volt negative bias, magnetizing current is by 500,400,300mA changes successively, sputtering current is 300-500mA, each magnetizing current cleans 10-30min, guarantees that the natural oxide film on aluminium target surface is removed by sputter clean, and the purity of aluminium target is 99.99%, a baffle plate is placed at 1-5cm place, aluminium target the place ahead in cleaning process, stop al deposition that sputter produces to the silver coin surface, clean end after, will carry on the back end vacuum again and take out and cause 0.005Pa;
The deposition of invisible protective layer of alumina: silver coin is heated to 300-400 ℃, removes the baffle plate in aluminium target the place ahead, feed Ar gas and O to vacuum chamber
2Oxygen mixture, gas flow ratio is 10: 1-20: 1, make gas pressure in vacuum between 0.2-0.5Pa, on magnetron sputtering target, apply a 300-1000 volt negative bias, magnetizing current transfers to 300-500mA, sputtering current is 300-500mA, and depositing time is 1-3min, applies the negative bias of a 50-100V in deposition process on the silver coin;
The aftertreatment of aluminium target: the aluminium target uses after 1-5 time, the aluminium target is unloaded, with 1000-3000# waterproof abrasive paper at the pre-grinding machine upthrow of metallographic light 5-10min, remove the alumina layer on aluminium target surface, use dehydrated alcohol ultrasonic cleaning 1-3 time again, each 2-10min, clean for the second time finish after with aluminium target hot blast drying.
Advantageous effect of the present invention is as follows:
The present invention has formed protective layer of alumina by above-mentioned steps on the surface of silverware especially silver coin, has kept the surface anti-discolouring of the metal-like of silver coin and silver coin, protective layer invisible, has guaranteed that effectively the visual appearance of silver coin and guard time are long.Technological operation of the present invention is simple, and cost is low, is fit to apply.
In addition, to blank silver coin and the silver coin establishing criteria BS EN ISO 4538:1995 that handled.Metallic coatings-Thioacetamide corrosion test (TAA test) has carried out the acceleration discoloration test.
After 15h was carried out in test, blank silver coin surface became golden yellow, loses the gloss of original argent, and the silver coin after the inventive method is handled does not have considerable change.After test proceeded to 120h, blank silver coin became sorrel, and there is slight tarnishing on the silver coin surface after the present invention handles.Therefore illustrate that the silver coin of handling through the inventive method has excellent discoloration-resisting.
Embodiment
Embodiment 1
The preparation method of the invisible anti-discolouring protective layer of silver coin surface alumina oxide realizes by following steps: the cleaning of (one) silver coin: at ambient temperature, with silver coin ultrasonic cleaning 2 times in dehydrated alcohol, each 5min, clean for the second time finish after with the silver coin hot blast drying; (2) silver coin is put into vacuum chamber, back of the body end vacuum is taken out and is caused 0.005Pa; (3) cleaning of aluminium target: feeding purity to vacuum chamber is 99.99% high-purity Ar gas, making air pressure is 0.4Pa, on magnetron sputtering target, apply 700 volts of negative biass, magnetizing current is by 500,400,300mA changes successively, sputtering current is 400mA, each magnetizing current cleans 20min, guarantees that the natural oxide film on aluminium target surface is removed by sputter clean, and the purity of aluminium target is 99.99%, a baffle plate is placed at 2cm place, aluminium target the place ahead in cleaning process, stop al deposition that sputter produces to the silver coin surface, clean end after, will carry on the back end vacuum again and take out and cause 0.005Pa; (4) deposition of invisible protective layer of alumina: silver coin is heated to 400 ℃, removes the baffle plate in aluminium target the place ahead, feed Ar gas and O to vacuum chamber
2Oxygen mixture, gas flow ratio is 10: 1, making gas pressure in vacuum is 0.3Pa, apply 600 volts of negative biass on magnetron sputtering target, magnetizing current transfers to 500mA, and sputtering current is 400mA, depositing time is 1min, applies the negative bias of a 50V in deposition process on the silver coin; (5) aluminium target aftertreatment: the aluminium target uses after 3 times, the aluminium target be unloaded, and uses 2000# waterproof abrasive paper at the pre-grinding machine upthrow of metallographic light 5min, remove the alumina layer on aluminium target surface, use the dehydrated alcohol ultrasonic cleaning again 2 times, each 5min, clean for the second time finish after with aluminium target hot blast drying.
Embodiment 2
The difference of this implementation step and embodiment 1 is the deposition of the invisible protective layer of alumina of implementation step (four): silver coin is heated to 300 ℃, removes the baffle plate in aluminium target the place ahead, feed Ar gas and O to vacuum chamber
2Oxygen mixture, gas flow ratio is 10: 1, making gas pressure in vacuum is 0.3Pa, apply 300 volts of negative biass on magnetron sputtering target, magnetizing current transfers to 500mA, and sputtering current is 400mA, depositing time is 1min, applies the negative bias of a 50V in deposition process on the silver coin.Other step is identical with embodiment 1.
Embodiment 3
The difference of this implementation step and embodiment 1 is the deposition of the invisible protective layer of alumina of implementation step (four): silver coin is heated to 400 ℃, removes the baffle plate in aluminium target the place ahead, feed Ar gas and O to vacuum chamber
2Oxygen mixture, gas flow ratio is 10: 1, making gas pressure in vacuum is 0.3Pa, apply 1000 volts of negative biass on magnetron sputtering target, magnetizing current transfers to 500mA, and sputtering current is 400mA, depositing time is 3min, applies the negative bias of a 50V in deposition process on the silver coin.Other step is identical with embodiment 1.
Embodiment 4
The difference of this implementation step and embodiment 1 is the deposition of the invisible protective layer of alumina of implementation step (four): silver coin is heated to 400 ℃, removes the baffle plate in aluminium target the place ahead, feed Ar gas and O to vacuum chamber
2Oxygen mixture, gas flow ratio is 10: 1, making gas pressure in vacuum is 0.3Pa, apply 500 volts of negative biass on magnetron sputtering target, magnetizing current transfers to 500mA, and sputtering current is 400mA, depositing time is 2min, applies the negative bias of a 100V in deposition process on the silver coin.Other step is identical with specific embodiment 1.
Embodiment 5
The difference of this implementation step and embodiment 1 is the deposition of the invisible protective layer of alumina of implementation step (four): silver coin is heated to 400 ℃, removes the baffle plate in aluminium target the place ahead, feed Ar gas and O to vacuum chamber
2Oxygen mixture, gas flow ratio is 20: 1, making gas pressure in vacuum is 0.3Pa, apply 800 volts of negative biass on magnetron sputtering target, magnetizing current transfers to 500mA, and sputtering current is 400mA, depositing time is 2min, applies the negative bias of a 50V in deposition process on the silver coin.Other step is identical with specific embodiment 1.
Embodiment 6
The difference of this implementation step and embodiment one is the deposition of the invisible protective layer of alumina of implementation step (four): silver coin is heated to 400 ℃, removes the baffle plate in aluminium target the place ahead, feed Ar gas and O to vacuum chamber
2Oxygen mixture, gas flow ratio is 10: 1, making gas pressure in vacuum is 0.2Pa, apply 400 volts of negative biass on magnetron sputtering target, magnetizing current transfers to 500mA, and sputtering current is 400mA, depositing time is 1min, applies the negative bias of a 50V in deposition process on the silver coin.Other step is identical with specific embodiment one.
Embodiment 7
The difference of this implementation step and embodiment 1 is the deposition of the invisible protective layer of alumina of implementation step (four): silver coin is heated to 300 ℃, removes the baffle plate in aluminium target the place ahead, feed Ar gas and O to vacuum chamber
2Oxygen mixture, gas flow ratio is 10: 1, making gas pressure in vacuum is 0.2Pa, apply 900 volts of negative biass on magnetron sputtering target, magnetizing current transfers to 500mA, and sputtering current is 400mA, depositing time is 1min, applies the negative bias of a 50V in deposition process on the silver coin.Other step is identical with specific embodiment 1.
Embodiment 8
The cleaning of silver coin: at ambient temperature, with silver coin ultrasonic cleaning 1 time in dehydrated alcohol, each 10min, clean for the second time finish after with the silver coin hot blast drying;
Vacuumize: silver coin is put into vacuum chamber, and back of the body end vacuum is taken out and is caused 0.005Pa;
The cleaning of aluminium target: feeding purity to vacuum chamber is 99.99% high-purity Ar gas, make air pressure at 0.2Pa, on magnetron sputtering target, apply 300 volts of negative biass, magnetizing current is by 500,400,300mA changes successively, sputtering current is 300mA, each magnetizing current cleans 30min, guarantees that the natural oxide film on aluminium target surface is removed by sputter clean, and the purity of aluminium target is 99.99%, a baffle plate is placed at 1cm place, aluminium target the place ahead in cleaning process, stop al deposition that sputter produces to the silver coin surface, clean end after, will carry on the back end vacuum again and take out and cause 0.005Pa;
The deposition of invisible protective layer of alumina: silver coin is heated to 300 ℃, removes the baffle plate in aluminium target the place ahead, feed Ar gas and O to vacuum chamber
2Oxygen mixture, gas flow ratio is 10: 1, makes gas pressure in vacuum at 0.2Pa, apply 300 volts of negative biass on magnetron sputtering target, magnetizing current transfers to 300mA, and sputtering current is 300mA, depositing time is 3min, applies the negative bias of a 50V in deposition process on the silver coin;
The aftertreatment of aluminium target: the aluminium target uses after 1 time, and the aluminium target is unloaded, and uses 3000# waterproof abrasive paper at the pre-grinding machine upthrow of metallographic light 10min, remove the alumina layer on aluminium target surface, use the dehydrated alcohol ultrasonic cleaning again 1 time, each 10min, clean for the second time finish after with aluminium target hot blast drying.
Embodiment 9
The cleaning of silver coin: at ambient temperature, with silver coin ultrasonic cleaning 3 times in dehydrated alcohol, each 2min, clean for the second time finish after with the silver coin hot blast drying;
Vacuumize: silver coin is put into vacuum chamber, and back of the body end vacuum is taken out and is caused 0.005Pa;
The cleaning of aluminium target: feeding purity to vacuum chamber is 99.99% high-purity Ar gas, make air pressure at 0.5Pa, on magnetron sputtering target, apply 1000 volts of negative biass, magnetizing current is by 500,400,300mA changes successively, sputtering current is 500mA, each magnetizing current cleans 30min, guarantees that the natural oxide film on aluminium target surface is removed by sputter clean, and the purity of aluminium target is 99.99%, a baffle plate is placed at 5cm place, aluminium target the place ahead in cleaning process, stop al deposition that sputter produces to the silver coin surface, clean end after, will carry on the back end vacuum again and take out and cause 0.005Pa;
The deposition of invisible protective layer of alumina: silver coin is heated to 400 ℃, removes the baffle plate in aluminium target the place ahead, feed Ar gas and O to vacuum chamber
2Oxygen mixture, gas flow ratio is 20: 1, makes gas pressure in vacuum at 0.5Pa, apply 1000 volts of negative biass on magnetron sputtering target, magnetizing current transfers to 500mA, and sputtering current is 500mA, depositing time is 1min, applies the negative bias of a 100V in deposition process on the silver coin;
The aftertreatment of aluminium target: the aluminium target uses after 5 times, and the aluminium target is unloaded, and uses 1000# waterproof abrasive paper at the pre-grinding machine upthrow of metallographic light 5min, remove the alumina layer on aluminium target surface, use the dehydrated alcohol ultrasonic cleaning again 3 times, each 2min, clean for the second time finish after with aluminium target hot blast drying.
Claims (4)
1. a silver coin is characterized in that the outside surface of silver coin is provided with invisible anti-discolouring protective layer of alumina.
2. a preparation method who prepares the described silver coin of claim 1 is characterized in that comprising the steps:
The cleaning of silver coin: at ambient temperature, with silver coin ultrasonic cleaning 2 times in dehydrated alcohol, each 2-10min, clean for the second time finish after with the silver coin hot blast drying;
Vacuumize: silver coin is put into vacuum chamber, and back of the body end vacuum is evacuated to 0.005Pa;
The cleaning of aluminium target: feeding purity to vacuum chamber is 99.99% high-purity Ar gas, make air pressure between 0.2-0.5Pa, on magnetron sputtering target, apply a 300-1000 volt negative bias, magnetizing current is by 500,400,300mA changes successively, sputtering current is 300-500mA, each magnetizing current cleans 10-30min, guarantees that the natural oxide film on aluminium target surface is removed by sputter clean, and the purity of aluminium target is 99.99%, a baffle plate is placed at 1-5cm place, aluminium target the place ahead in cleaning process, the al deposition that stops the sputter generation is to the silver coin surface, and cleaning will be carried on the back end vacuum again and be evacuated to 0.005Pa after being finished;
The deposition of invisible protective layer of alumina: silver coin is heated to 300-400 ℃, removes the baffle plate in aluminium target the place ahead, feed Ar gas and O to vacuum chamber
2Oxygen mixture, gas flow ratio is 10: 1-20: 1, make gas pressure in vacuum between 0.2-0.5Pa, on magnetron sputtering target, apply a 300-1000 volt negative bias, magnetizing current transfers to 300-500mA, sputtering current is 300-500mA, and depositing time is 1-3min, applies the negative bias of a 50-100V in deposition process on the silver coin;
The aftertreatment of aluminium target: the aluminium target uses after 1-5 time, and the aluminium target is unloaded, and uses 1000-3000# waterproof abrasive paper at the pre-grinding machine upthrow of metallographic light 5-10min, remove the alumina layer on aluminium target surface, use the dehydrated alcohol ultrasonic cleaning again 2 times, each 2-10min, clean for the second time finish after with aluminium target hot blast drying.
3. the preparation method of silver coin according to claim 2 is characterized in that comprising the steps:
The cleaning of silver coin: at ambient temperature, with silver coin ultrasonic cleaning 2 times in dehydrated alcohol, each 5min, clean for the second time finish after with the silver coin hot blast drying;
Vacuumize: silver coin is put into vacuum chamber, and back of the body end vacuum is evacuated to 0.005Pa;
The cleaning of aluminium target: feeding purity to vacuum chamber is 99.99% high-purity Ar gas, make air pressure between 0.2-0.5Pa, on magnetron sputtering target, apply a 300-1000 volt negative bias, magnetizing current is by 500,400,300mA changes successively, sputtering current is 400mA, each magnetizing current cleans 10-30min, guarantees that the natural oxide film on aluminium target surface is removed by sputter clean, and the purity of aluminium target is 99.99%, a baffle plate is placed at 2cm place, aluminium target the place ahead in cleaning process, the al deposition that stops the sputter generation is to the silver coin surface, and cleaning will be carried on the back end vacuum again and be evacuated to 0.005Pa after being finished;
The deposition of invisible protective layer of alumina: silver coin is heated to 300-400 ℃, removes the baffle plate in aluminium target the place ahead, feed Ar gas and O to vacuum chamber
2Oxygen mixture, gas flow ratio is 10: 1-20: 1, make gas pressure in vacuum between 0.2-0.5Pa, on magnetron sputtering target, apply a 300-1000 volt negative bias, magnetizing current transfers to 500mA, sputtering current is 400mA, and depositing time is 1-3min, applies the negative bias of a 50-100V in deposition process on the silver coin;
The aftertreatment of aluminium target: the aluminium target uses after 3 times, and the aluminium target is unloaded, and uses 2000# waterproof abrasive paper at the pre-grinding machine upthrow of metallographic light 5-10min, remove the alumina layer on aluminium target surface, use the dehydrated alcohol ultrasonic cleaning again 2 times, each 5min, clean for the second time finish after with aluminium target hot blast drying.
4. the preparation method of silver coin according to claim 2 is characterized in that comprising the steps:
The cleaning of silver coin: at ambient temperature, with silver coin ultrasonic cleaning 2 times in dehydrated alcohol, each 5min, clean for the second time finish after with the silver coin hot blast drying;
Vacuumize: silver coin is put into vacuum chamber, and back of the body end vacuum is evacuated to 0.005Pa;
The cleaning of aluminium target: feeding purity to vacuum chamber is 99.99% high-purity Ar gas, making air pressure is 0.4Pa, on magnetron sputtering target, apply 700 volts of negative biass, magnetizing current is by 500,400,300mA changes successively, sputtering current is 400mA, each magnetizing current cleans 20min, guarantees that the natural oxide film on aluminium target surface is removed by sputter clean, and the purity of aluminium target is 99.99%, a baffle plate is placed at 2cm place, aluminium target the place ahead in cleaning process, the al deposition that stops the sputter generation is to the silver coin surface, and cleaning will be carried on the back end vacuum again and be evacuated to 0.005Pa after being finished;
The deposition of invisible protective layer of alumina: silver coin is heated to 400 ℃, removes the baffle plate in aluminium target the place ahead, feed Ar gas and O to vacuum chamber
2Oxygen mixture, gas flow ratio is 10: 1, making gas pressure in vacuum is 0.3Pa, apply 600 volts of negative biass on magnetron sputtering target, magnetizing current transfers to 500mA, and sputtering current is 400mA, depositing time is 1min, applies the negative bias of a 50V in deposition process on the silver coin;
The aftertreatment of aluminium target: the aluminium target uses after 3 times, the aluminium target be unloaded, and uses 2000# waterproof abrasive paper at the pre-grinding machine upthrow of metallographic light 5min, remove the alumina layer on aluminium target surface, use the dehydrated alcohol ultrasonic cleaning again 2 times, each 5min, clean for the second time finish after with aluminium target hot blast drying.
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| CN110158064B (en) * | 2019-07-02 | 2021-06-25 | 郴州市金贵银业股份有限公司 | Antioxidant silver and preparation method thereof |
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