CN109881173B - Process for forming metal composite layer on silver-plated nylon surface and product thereof - Google Patents
Process for forming metal composite layer on silver-plated nylon surface and product thereof Download PDFInfo
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Abstract
The invention relates to the technical field of nylon processing, in particular to a process for forming a metal composite layer on the surface of silver-plated nylon and a product thereof. A process for forming a metal composite layer on the surface of silver-plated nylon comprises the following steps: and depositing an alloy layer on the surface of the nylon containing the silver layer by adopting a magnetron sputtering method to obtain the nylon containing the metal composite layer. The nylon prepared by the method has good surface flatness, has a positive effect on later nylon processing application, and the nylon product prepared by the process has good infrared radiation blocking performance, plays a role in heat insulation and warmth retention, is used in space shuttles, missiles and the like, is light, high in strength, does not discolor and is durable, and a novel silver-plated space antenna material and a flexible electrode material are provided. When the fabric is used in textiles, the fabric has the effects of being warm in winter and cool in summer, and the visibility of the color and the texture of the fabric cannot be reduced, so that the color and the texture of the fabric have better effects.
Description
Technical Field
The invention belongs to the technical field of nylon processing, and particularly relates to a process for forming a metal composite layer on the surface of silver-plated nylon and a product thereof.
Background
Under the continuous irradiation of sunlight, objects accumulate a large amount of heat, particularly in hot summer, so that the internal temperature of the objects is increased, and inconvenience and harm are brought to production and life of people. With the improvement of living standard of people, outdoor activities are more and more popular, the existing outdoor textile does not have good blocking effect on infrared radiation accounting for 46% of solar energy in sunlight, and in order to reduce troubles brought to production and living of people by high-temperature environment, the outdoor textile with the infrared reflection function is needed. The nylon surface is coated with a film layer capable of reflecting infrared rays, so that infrared radiation emitted by the sun can be blocked in a hot environment, and meanwhile, the infrared radiation loss of the covering in the nylon can be reduced in cold winter, so that the requirements on heat insulation and heat preservation are met. The outdoor textile made of the nylon becomes a new solution for heat insulation and warm keeping which can be widely applied.
The metal silver has a very good infrared reflection function, and the larger the thickness of the film layer is, the better the infrared reflection effect is. However, the silver film layer is easily oxidized in the coating process, so that the flatness is reduced, the thickness of the silver film layer on the surface of the nylon is not uniform, and the transmission of visible light is exponentially reduced when the thickness is too high, so that the visibility of the color and the texture of the fabric is reduced, and imperfect use effect is brought to people.
Disclosure of Invention
In order to solve the problems, the invention provides a process for forming a metal composite layer on the surface of silver-plated nylon, which comprises the following steps: and depositing an alloy layer on the surface of the nylon containing the silver layer to obtain the nylon containing the metal composite layer.
As a preferable technical scheme, the nylon containing the metal composite layer is formed by one or more of a vacuum evaporation technology, a metal organic chemical vapor deposition method, a pulse laser deposition method, a spray pyrolysis method, a molecular beam epitaxy method, plasma spraying, a multi-arc ion vacuum coating technology, an optical vacuum coating technology, other vacuum coating and chemical silver plating.
As a preferable technical scheme, the method comprises the following steps:
s01: depositing a first silver layer on the surface of the nylon by adopting a chemical silver plating method to obtain the nylon containing the first silver layer;
s02: and depositing a second alloy layer on the surface of the nylon containing the first silver layer by adopting a magnetron sputtering method to obtain the nylon containing the metal composite layer.
As a preferred technical scheme, the second alloy layer is composed of one or more elements of Ti, Al, Au, In, Ga, Se, La, Ce, Fe, Zn, Cu, W, Mg, Cr, Ni, V, Co and Pt.
As a preferable technical scheme, the second alloy layer is AZO (ZnO: Al)2O3) A transparent conductive thin film layer.
As a preferable technical solution, the second alloy layer is an ITO thin film layer.
As a preferable technical solution, the targets assembled in the vacuum sputtering chamber in the magnetron sputtering method in step S02 include a metal target and a ceramic target.
As a preferred technical scheme, the metal target comprises a metal titanium target, a metal aluminum target, a metal silver target, a metal zinc target, a metal tin target, an alloy zinc tin target and an alloy titanium aluminum target; the ceramic target comprises a titanium oxide ceramic target, a silicon aluminum target, an AZO ceramic target, an iron oxide ceramic target and an ITO ceramic target.
As a preferable technical scheme, the target is a plane target, a direct current power supply is connected, and the sputtering power is 1-40 kW.
As a preferred technical solution, the deposition atmosphere in the vacuum sputtering chamber includes argon and krypton.
Has the advantages that: the nylon prepared by the method has good surface flatness, has a positive effect on later-stage nylon processing application, and the nylon product prepared by the process has good infrared radiation blocking performance, plays a role in heat insulation and warmth retention, is widely applied, and can be used in textiles, so that the fabric has the effects of being warm in winter and cool in summer, and the visibility of the color and the texture of the fabric can not be reduced, thereby the color and the texture of the fabric have good effects.
Detailed Description
The technical features of the technical solutions provided by the present invention are further clearly and completely described below with reference to the specific embodiments, and the scope of protection is not limited thereto.
The words "preferred", "more preferred", and the like, in the present invention refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
In order to solve the problems, the invention provides a process for forming a metal composite layer on the surface of silver-plated nylon, which comprises the following steps: and depositing an alloy layer on the surface of the nylon containing the silver layer to obtain the nylon containing the metal composite layer.
In a preferred embodiment, the nylon containing the metal composite layer is formed by one or more of vacuum evaporation technology, metallorganic chemical vapor deposition, pulsed laser deposition, spray pyrolysis, molecular beam epitaxy, plasma spraying, multi-arc ion vacuum coating, optical vacuum coating, other vacuum coating, and electroless silver coating.
As a preferable technical scheme, the method comprises the following steps:
s01: depositing a first silver layer on the surface of the nylon by adopting a chemical silver plating method to obtain the nylon containing the first silver layer;
s02: and depositing a second alloy layer on the surface of the nylon containing the first silver layer by adopting a magnetron sputtering method to obtain the nylon containing the metal composite layer.
First silver layer
In some embodiments, the electroless silver plating method in step S01 of the present invention comprises:
(1) washing: cleaning the nylon surface by using water and a detergent to remove oil stains and impurities;
(2) coarsening: placing the cleaned nylon in a chemical coarsening solution, soaking for 10-30min at 20-40 ℃, and then washing with clear water;
(3) sensitization: soaking the cleaned nylon in hydrochloric acid water solution containing stannous chloride at 20-40 deg.c for 10-30min and washing with clear water;
(4) chemical silver plating: and (3) placing the sensitized nylon into silver plating reaction liquid, stirring the solution at room temperature for 1min to obtain a mixed solution, then adding sodium tartrate and sodium itaconate into the mixed solution, raising the temperature to 70 ℃, cooling the temperature to room temperature after 30min, then raising the temperature to 70 ℃, repeating the steps of raising the temperature and cooling for three times, and taking out the nylon to obtain the nylon containing the first silver layer.
In a preferred embodiment, in step (2) of the present invention: the concentration of nylon in the chemical roughening solution is 20 wt%, the chemical roughening solution is a mixed solution containing ascorbic acid, sodium hydroxide, hexadecyl trimethyl ammonium bromide and water, and the mass ratio of the ascorbic acid, the sodium hydroxide, the hexadecyl trimethyl ammonium bromide and the water is (0.01-0.06): (0.02-0.08): (0.02-0.1): 1, more preferably, the mass ratio of the ascorbic acid, the sodium hydroxide, the hexadecyl trimethyl ammonium bromide and the water is 0.05: 0.06: 0.05: 1.
in a preferred embodiment, in step (3) of the present invention: the concentration of nylon in the hydrochloric acid aqueous solution containing stannous chloride is 30 wt%, and the mass ratio of the stannous chloride to the concentrated hydrochloric acid to the water in the hydrochloric acid aqueous solution containing stannous chloride is (0.02-0.05): (0.02-0.06): 1, more preferably, the mass ratio of the stannous chloride to the concentrated hydrochloric acid to the water is 0.03: 0.04: 1.
in a preferred embodiment, in step (4) of the present invention: the silver plating reaction liquid is a mixed solution containing silver nitrate, ammonia water, potassium hydroxide and ethanol, and the mass ratio of the silver nitrate to the ammonia water to the potassium hydroxide to the ethanol is (0.2-0.5): (0.4-0.8): (0.05-0.1): 1, more preferably, the mass ratio of the silver nitrate to the ammonia water to the potassium hydroxide to the ethanol is 0.3: 0.6: 0.06: 1.
in a preferred embodiment, in step (4) of the present invention: the concentration of nylon in the silver-plating reaction liquid is 25 wt%, the total concentration of sodium tartrate and sodium itaconate in the silver-plating reaction liquid is 2 wt% -10 wt%, and the molar ratio of the sodium tartrate to the sodium itaconate is 1 (0.6-1.2); more preferably, the total concentration of sodium tartrate and sodium itaconate in the silver plating reaction liquid is 5 wt%, and the molar ratio of sodium tartrate to sodium itaconate is 1:1.
The applicant has surprisingly found that when sodium tartrate and sodium itaconate are added to produce a nylon comprising a first silver layer, the deposited silver film has a higher flatness. The inventors speculate that the possible reason is that the addition of both helps the reduction of silver, acting as a nucleus, while the four carbons on the sodium tartrate can form four points of crystal growth, which is beneficial to the rapid growth of silver. Meanwhile, under the coordination of sodium itaconate, under the concave area, the points of sodium tartrate are redundant of the convex area, so that the growth of silver is more selective. In addition, the inventor also finds that the effect on the effect is better when the molar ratio of the sodium tartrate to the sodium itaconate is 1 (0.6-1.2), and the inventor speculates that four carbons on the sodium tartrate can form four points of crystal growth, and two hydroxyl groups on the sodium itaconate have certain chelation, so that the silver forming is accelerated.
Second alloy layer
In a preferred embodiment, the second alloy layer of the present invention is deposited by magnetron sputtering.
The magnetron sputtering method of the invention is to fill a proper amount of argon gas into high vacuum, apply a direct current voltage of hundreds of K between a cathode (a columnar target or a plane target) and an anode (a coating chamber wall), generate magnetic control type abnormal glow discharge in a coating chamber and ionize the argon gas; the argon ions are accelerated by the cathode and bombard the surface of the cathode target, and atoms on the surface of the target are sputtered out to deposit on the surface of the substrate to form a film.
In some embodiments, the second alloy layer is composed of one or more elements selected from Ti, Al, Au, In, Ga, Se, La, Ce, Fe, Zn, Cu, W, Mg, Cr, Ni, V, Co, and Pt.
In some embodiments, the target material assembled in the vacuum sputtering chamber in the magnetron sputtering method of the present invention comprises a metal target material; the metal target comprises a metal titanium target, a metal aluminum target, a metal silver target, a metal zinc target, a metal tin target, an alloy zinc tin target and an alloy titanium aluminum target.
In some embodiments, the deposition atmosphere within the vacuum sputtering chamber of the present invention comprises argon, krypton.
In some embodiments, the target material in the vacuum sputtering chamber is a planar target, and is connected to a direct current power supply, and the sputtering power is 1 to 40 kW.
In some embodiments, the second alloy layer of the present invention is deposited by a magnetron sputtering method, comprising: and placing the nylon containing the first silver layer in a continuous vacuum sputtering cavity for magnetron sputtering film formation, depositing a second alloy layer in the sputtering cavity, wherein the target is any one of an alloy titanium aluminum target, an ITO ceramic target and an AZO ceramic target, the atmosphere is pure argon, the air pressure is 0.5-1Pa, the sputtering power of a direct-current power supply is 7-12kW, and the thickness of the second alloy layer is controlled to be 1-15nm, so that the nylon containing the metal composite layer is obtained.
In a preferred embodiment, the second alloy layer of the present invention is a titanium aluminum alloy layer.
In a preferred embodiment, the second alloy layer of the present invention is deposited by a magnetron sputtering method, and the method comprises the steps of: putting the nylon containing the first silver layer into a continuous vacuum sputtering cavity for magnetron sputtering film formation, depositing a second alloy layer in the sputtering cavity, wherein the target material is an alloy titanium aluminum target, the atmosphere is pure argon, the air pressure is 0.5Pa, the sputtering power of a direct-current power supply is 9kW, and the thickness of the second alloy layer is controlled to be 8nm, so that the nylon containing the metal composite layer is obtained.
In a preferred embodiment, the second alloy layer of the present invention is AZO (ZnO: Al)2O3) A transparent conductive thin film layer.
In a preferred embodiment, the second alloy layer of the present invention is deposited by a magnetron sputtering method, and the method comprises the steps of: and placing the nylon containing the first silver layer in a continuous vacuum sputtering cavity for magnetron sputtering film formation, depositing a second alloy layer in the sputtering cavity, wherein the target material is an AZO ceramic target, the atmosphere is pure argon, the air pressure is 0.5Pa, the sputtering power of a direct-current power supply is 9kW, and the thickness of the second alloy layer is controlled to be 8nm, so that the nylon containing the metal composite layer is obtained.
In a preferred embodiment, the second alloy layer of the present invention is an ITO thin film layer.
In a preferred embodiment, the second alloy layer of the present invention is deposited by a magnetron sputtering method, and the method comprises the steps of: putting the nylon containing the first silver layer into a continuous vacuum sputtering cavity for magnetron sputtering film formation, depositing a second alloy layer in the sputtering cavity, wherein the target material is an ITO ceramic target, the atmosphere is pure argon, the air pressure is 0.5Pa, the sputtering power of a direct-current power supply is 9kW, and the thickness of the second alloy layer is controlled to be 8nm, so that the nylon containing the metal composite layer is obtained.
The invention provides the application of the nylon containing the metal composite layer in fabrics, non-woven fabrics, artificial leather, sponges, plastic films, flexible materials, clothes and bedding.
The present invention will now be described in detail by way of examples, and the starting materials used are commercially available unless otherwise specified.
Examples
Example 1
Embodiment 1 provides a process for forming a metal composite layer on a silver-plated nylon surface, comprising the following steps:
s01: depositing a first silver layer on the surface of the nylon by adopting a chemical silver plating method to obtain the nylon containing the first silver layer;
s02: and depositing a second alloy layer on the surface of the nylon containing the first silver layer by adopting a magnetron sputtering method to obtain the nylon containing the metal composite layer.
The first silver layer is deposited by a chemical silver plating method and comprises the following steps:
(1) washing: cleaning the nylon surface by using water and a detergent to remove oil stains and impurities;
(2) coarsening: placing the cleaned nylon in a chemical coarsening solution, soaking for 10-30min at 20-40 ℃, and then washing with clear water;
(3) sensitization: soaking the cleaned nylon in hydrochloric acid water solution containing stannous chloride at 20-40 deg.c for 10-30min and washing with clear water;
(4) chemical silver plating: and (3) placing the sensitized nylon into silver plating reaction liquid, stirring the solution at room temperature for 1min to obtain a mixed solution, then adding sodium tartrate and sodium itaconate into the mixed solution, raising the temperature to 70 ℃, cooling the temperature to room temperature after 30min, then raising the temperature to 70 ℃, repeating the steps of raising the temperature and cooling for three times, and taking out the nylon to obtain the nylon containing the first silver layer.
Wherein in the step (2): the concentration of nylon in the chemical roughening solution is 20 wt%, the chemical roughening solution is a mixed solution containing ascorbic acid, sodium hydroxide, hexadecyl trimethyl ammonium bromide and water, and the mass ratio of the ascorbic acid to the sodium hydroxide to the hexadecyl trimethyl ammonium bromide to the water is 0.05: 0.06: 0.05: 1.
in the step (3): the concentration of nylon in the hydrochloric acid aqueous solution containing stannous chloride is 30 wt%, and the mass ratio of the stannous chloride to the concentrated hydrochloric acid to the water is 0.03: 0.04: 1.
in the step (4): the silver plating reaction liquid is a mixed solution containing silver nitrate, ammonia water, potassium hydroxide and ethanol, and the mass ratio of the silver nitrate to the ammonia water to the potassium hydroxide to the ethanol is 0.3: 0.6: 0.06: 1; the concentration of nylon in the silver plating reaction liquid is 25 wt%, the total concentration of sodium tartrate and sodium itaconate in the silver plating reaction liquid is 5 wt%, and the molar ratio of the sodium tartrate to the sodium itaconate is 1:1.
The second alloy layer is deposited by a magnetron sputtering method and comprises the following steps: and placing the nylon containing the first silver layer in a continuous vacuum sputtering cavity for magnetron sputtering film formation, depositing a second alloy layer in the sputtering cavity, wherein the target material is an alloy titanium aluminum target, the atmosphere is pure argon, the air pressure is 0.5Pa, the sputtering power of a direct-current power supply is 9kW, and the thickness of the second alloy layer is controlled to be 8nm, so that the nylon containing the metal composite layer is obtained.
Example 2
Embodiment 2 provides a process for forming a metal composite layer on a silver-plated nylon surface, which comprises the following steps:
s01: depositing a first silver layer on the surface of the nylon by adopting a chemical silver plating method to obtain the nylon containing the first silver layer;
s02: and depositing a second alloy layer on the surface of the nylon containing the first silver layer by adopting a magnetron sputtering method to obtain the nylon containing the metal composite layer.
The first silver layer is deposited by a chemical silver plating method and comprises the following steps:
(1) washing: cleaning the nylon surface by using water and a detergent to remove oil stains and impurities;
(2) coarsening: placing the cleaned nylon in a chemical coarsening solution, soaking for 10-30min at 20-40 ℃, and then washing with clear water;
(3) sensitization: soaking the cleaned nylon in hydrochloric acid water solution containing stannous chloride at 20-40 deg.c for 10-30min and washing with clear water;
(4) chemical silver plating: and (3) placing the sensitized nylon into silver plating reaction liquid, stirring the solution at room temperature for 1min to obtain a mixed solution, then adding sodium tartrate and sodium itaconate into the mixed solution, raising the temperature to 70 ℃, cooling the temperature to room temperature after 30min, then raising the temperature to 70 ℃, repeating the steps of raising the temperature and cooling for three times, and taking out the nylon to obtain the nylon containing the first silver layer.
Wherein in the step (2): the concentration of nylon in the chemical roughening solution is 20 wt%, the chemical roughening solution is a mixed solution containing ascorbic acid, sodium hydroxide, hexadecyl trimethyl ammonium bromide and water, and the mass ratio of the ascorbic acid to the sodium hydroxide to the hexadecyl trimethyl ammonium bromide to the water is 0.05: 0.06: 0.05: 1.
in the step (3): the concentration of nylon in the hydrochloric acid aqueous solution containing stannous chloride is 30 wt%, and the mass ratio of the stannous chloride to the concentrated hydrochloric acid to the water is 0.03: 0.04: 1.
in the step (4): the silver plating reaction liquid is a mixed solution containing silver nitrate, ammonia water, potassium hydroxide and ethanol, and the mass ratio of the silver nitrate to the ammonia water to the potassium hydroxide to the ethanol is 0.3: 0.6: 0.06: 1; the concentration of nylon in the silver plating reaction liquid is 25 wt%, the total concentration of sodium tartrate and sodium itaconate in the silver plating reaction liquid is 2 wt%, and the molar ratio of the sodium tartrate to the sodium itaconate is 1: 0.6.
The second alloy layer is deposited by a magnetron sputtering method and comprises the following steps: and placing the nylon containing the first silver layer in a continuous vacuum sputtering cavity for magnetron sputtering film formation, depositing a second alloy layer in the sputtering cavity, wherein the target material is an AZO ceramic target, the atmosphere is pure argon, the air pressure is 0.5Pa, the sputtering power of a direct-current power supply is 9kW, and the thickness of the second alloy layer is controlled to be 8nm, so that the nylon containing the metal composite layer is obtained.
Example 3
Embodiment 3 provides a process for forming a metal composite layer on a silver-plated nylon surface, comprising the following steps:
s01: depositing a first silver layer on the surface of the nylon by adopting a chemical silver plating method to obtain the nylon containing the first silver layer;
s02: and depositing a second alloy layer on the surface of the nylon containing the first silver layer by adopting a magnetron sputtering method to obtain the nylon containing the metal composite layer.
The first silver layer is deposited by a chemical silver plating method and comprises the following steps:
(1) washing: cleaning the nylon surface by using water and a detergent to remove oil stains and impurities;
(2) coarsening: placing the cleaned nylon in a chemical coarsening solution, soaking for 10-30min at 20-40 ℃, and then washing with clear water;
(3) sensitization: soaking the cleaned nylon in hydrochloric acid water solution containing stannous chloride at 20-40 deg.c for 10-30min and washing with clear water;
(4) chemical silver plating: and (3) placing the sensitized nylon into silver plating reaction liquid, stirring the solution at room temperature for 1min to obtain a mixed solution, then adding sodium tartrate and sodium itaconate into the mixed solution, raising the temperature to 70 ℃, cooling the temperature to room temperature after 30min, then raising the temperature to 70 ℃, repeating the steps of raising the temperature and cooling for three times, and taking out the nylon to obtain the nylon containing the first silver layer.
Wherein in the step (2): the concentration of nylon in the chemical roughening solution is 20 wt%, the chemical roughening solution is a mixed solution containing ascorbic acid, sodium hydroxide, hexadecyl trimethyl ammonium bromide and water, and the mass ratio of the ascorbic acid to the sodium hydroxide to the hexadecyl trimethyl ammonium bromide to the water is 0.05: 0.06: 0.05: 1.
in the step (3): the concentration of nylon in the hydrochloric acid aqueous solution containing stannous chloride is 30 wt%, and the mass ratio of the stannous chloride to the concentrated hydrochloric acid to the water is 0.03: 0.04: 1.
in the step (4): the silver plating reaction liquid is a mixed solution containing silver nitrate, ammonia water, potassium hydroxide and ethanol, and the mass ratio of the silver nitrate to the ammonia water to the potassium hydroxide to the ethanol is 0.3: 0.6: 0.06: 1; the concentration of nylon in the silver plating reaction liquid is 25 wt%, the total concentration of sodium tartrate and sodium itaconate in the silver plating reaction liquid is 10 wt%, and the molar ratio of the sodium tartrate to the sodium itaconate is 1: 1.2.
The second alloy layer is deposited by a magnetron sputtering method and comprises the following steps: putting the nylon containing the first silver layer into a continuous vacuum sputtering cavity for magnetron sputtering film formation, depositing a second alloy layer in the sputtering cavity, wherein the target material is an ITO ceramic target, the atmosphere is pure argon, the air pressure is 0.5Pa, the sputtering power of a direct-current power supply is 9kW, and the thickness of the second alloy layer is controlled to be 8nm, so that the nylon containing the metal composite layer is obtained.
Example 4
Embodiment 4 provides a process for forming a metal composite layer on a silver-plated nylon surface, comprising the following steps:
s01: depositing a first silver layer on the surface of the nylon by adopting a chemical silver plating method to obtain the nylon containing the first silver layer;
s02: and depositing a second alloy layer on the surface of the nylon containing the first silver layer by adopting a magnetron sputtering method to obtain the nylon containing the metal composite layer.
The first silver layer is deposited by a chemical silver plating method and comprises the following steps:
(1) washing: cleaning the nylon surface by using water and a detergent to remove oil stains and impurities;
(2) coarsening: placing the cleaned nylon in a chemical coarsening solution, soaking for 10-30min at 20-40 ℃, and then washing with clear water;
(3) sensitization: soaking the cleaned nylon in hydrochloric acid water solution containing stannous chloride at 20-40 deg.c for 10-30min and washing with clear water;
(4) chemical silver plating: and (3) placing the sensitized nylon into silver plating reaction liquid, stirring the solution at room temperature for 1min to obtain a mixed solution, then adding sodium tartrate and sodium itaconate into the mixed solution, raising the temperature to 70 ℃, cooling the temperature to room temperature after 30min, then raising the temperature to 70 ℃, repeating the steps of raising the temperature and cooling for three times, and taking out the nylon to obtain the nylon containing the first silver layer.
Wherein in the step (2): the concentration of nylon in the chemical roughening solution is 20 wt%, the chemical roughening solution is a mixed solution containing ascorbic acid, sodium hydroxide, hexadecyl trimethyl ammonium bromide and water, and the mass ratio of the ascorbic acid to the sodium hydroxide to the hexadecyl trimethyl ammonium bromide to the water is 0.05: 0.06: 0.05: 1.
in the step (3): the concentration of nylon in the hydrochloric acid aqueous solution containing stannous chloride is 30 wt%, and the mass ratio of the stannous chloride to the concentrated hydrochloric acid to the water is 0.03: 0.04: 1.
in the step (4): the silver plating reaction liquid is a mixed solution containing silver nitrate, ammonia water, potassium hydroxide and ethanol, and the mass ratio of the silver nitrate to the ammonia water to the potassium hydroxide to the ethanol is 0.3: 0.6: 0.06: 1; the concentration of nylon in the silver-plating reaction liquid is 25 wt%, the total concentration of sodium tartrate and sodium itaconate in the silver-plating reaction liquid is 3 wt%, and the molar ratio of the sodium tartrate to the sodium itaconate is 1: 0.8.
The second alloy layer is deposited by a magnetron sputtering method and comprises the following steps: and placing the nylon containing the first silver layer in a continuous vacuum sputtering cavity for magnetron sputtering film formation, depositing a second alloy layer in the sputtering cavity, wherein the target material is an alloy titanium aluminum target, the atmosphere is pure argon, the air pressure is 0.5Pa, the sputtering power of a direct-current power supply is 9kW, and the thickness of the second alloy layer is controlled to be 8nm, so that the nylon containing the metal composite layer is obtained.
Example 5
Embodiment 5 provides a process for forming a metal composite layer on a silver-plated nylon surface, comprising the steps of:
s01: depositing a first silver layer on the surface of the nylon by adopting a chemical silver plating method to obtain the nylon containing the first silver layer;
s02: and depositing a second alloy layer on the surface of the nylon containing the first silver layer by adopting a magnetron sputtering method to obtain the nylon containing the metal composite layer.
The first silver layer is deposited by a chemical silver plating method and comprises the following steps:
(1) washing: cleaning the nylon surface by using water and a detergent to remove oil stains and impurities;
(2) coarsening: placing the cleaned nylon in a chemical coarsening solution, soaking for 10-30min at 20-40 ℃, and then washing with clear water;
(3) sensitization: soaking the cleaned nylon in hydrochloric acid water solution containing stannous chloride at 20-40 deg.c for 10-30min and washing with clear water;
(4) chemical silver plating: and (3) placing the sensitized nylon into silver plating reaction liquid, stirring the solution at room temperature for 1min to obtain a mixed solution, then adding sodium tartrate and sodium itaconate into the mixed solution, raising the temperature to 70 ℃, cooling the temperature to room temperature after 30min, then raising the temperature to 70 ℃, repeating the steps of raising the temperature and cooling for three times, and taking out the nylon to obtain the nylon containing the first silver layer.
Wherein in the step (2): the concentration of nylon in the chemical roughening solution is 20 wt%, the chemical roughening solution is a mixed solution containing ascorbic acid, sodium hydroxide, hexadecyl trimethyl ammonium bromide and water, and the mass ratio of the ascorbic acid to the sodium hydroxide to the hexadecyl trimethyl ammonium bromide to the water is 0.05: 0.06: 0.05: 1.
in the step (3): the concentration of nylon in the hydrochloric acid aqueous solution containing stannous chloride is 30 wt%, and the mass ratio of the stannous chloride to the concentrated hydrochloric acid to the water is 0.03: 0.04: 1.
in the step (4): the silver plating reaction liquid is a mixed solution containing silver nitrate, ammonia water, potassium hydroxide and ethanol, and the mass ratio of the silver nitrate to the ammonia water to the potassium hydroxide to the ethanol is 0.3: 0.6: 0.06: 1; the concentration of nylon in the silver plating reaction liquid is 25 wt%, the total concentration of sodium tartrate and sodium itaconate in the silver plating reaction liquid is 7 wt%, and the molar ratio of the sodium tartrate to the sodium itaconate is 1:1.
The second alloy layer is deposited by a magnetron sputtering method and comprises the following steps: and placing the nylon containing the first silver layer in a continuous vacuum sputtering cavity for magnetron sputtering film formation, depositing a second alloy layer in the sputtering cavity, wherein the target material is an alloy titanium aluminum target, the atmosphere is pure argon, the air pressure is 0.5Pa, the sputtering power of a direct-current power supply is 9kW, and the thickness of the second alloy layer is controlled to be 8nm, so that the nylon containing the metal composite layer is obtained.
Example 6
Embodiment 6 provides a process for forming a metal composite layer on a silver-plated nylon surface, comprising the steps of:
s01: depositing a first silver layer on the surface of the nylon by adopting a chemical silver plating method to obtain the nylon containing the first silver layer;
s02: and depositing a second alloy layer on the surface of the nylon containing the first silver layer by adopting a magnetron sputtering method to obtain the nylon containing the metal composite layer.
The first silver layer is deposited by a chemical silver plating method, and the steps are different from those of the embodiment 1 in that: and (4) the total concentration of the sodium tartrate and the sodium itaconate in the silver plating reaction liquid in the step (4) is 0 wt%.
The second alloy layer was deposited by magnetron sputtering, with the same procedure as in example 1.
Example 7
Embodiment 7 provides a process for forming a metal composite layer on a silver-plated nylon surface, comprising the steps of:
s01: depositing a first silver layer on the surface of the nylon by adopting a chemical silver plating method to obtain the nylon containing the first silver layer;
s02: and depositing a second alloy layer on the surface of the nylon containing the first silver layer by adopting a magnetron sputtering method to obtain the nylon containing the metal composite layer.
The first silver layer is deposited by a chemical silver plating method, and the steps are different from those of the embodiment 1 in that: the total concentration of the sodium tartrate and the sodium itaconate in the silver plating reaction liquid in the step (4) is 30 wt%.
The second alloy layer was deposited by magnetron sputtering, with the same procedure as in example 1.
Example 8
Embodiment 8 provides a process for forming a metal composite layer on a silver-plated nylon surface, comprising the steps of:
s01: depositing a first silver layer on the surface of the nylon by adopting a chemical silver plating method to obtain the nylon containing the first silver layer;
s02: and depositing a second alloy layer on the surface of the nylon containing the first silver layer by adopting a magnetron sputtering method to obtain the nylon containing the metal composite layer.
The first silver layer is deposited by a chemical silver plating method, and the steps are different from those of the embodiment 1 in that: in the step (4), the total concentration of sodium tartrate and sodium itaconate in the silver plating reaction liquid is 5 wt%, and the molar ratio of the sodium tartrate to the sodium itaconate is 1: 0.1.
The second alloy layer was deposited by magnetron sputtering, with the same procedure as in example 1.
Example 9
Embodiment 9 provides a process for forming a metal composite layer on a silver-plated nylon surface, comprising the steps of:
s01: depositing a first silver layer on the surface of the nylon by adopting a chemical silver plating method to obtain the nylon containing the first silver layer;
s02: and depositing a second alloy layer on the surface of the nylon containing the first silver layer by adopting a magnetron sputtering method to obtain the nylon containing the metal composite layer.
The first silver layer is deposited by a chemical silver plating method, and the steps are different from those of the embodiment 1 in that: in the step (4), the total concentration of sodium tartrate and sodium itaconate in the silver plating reaction liquid is 5 wt%, and the molar ratio of the sodium tartrate to the sodium itaconate is 1: 22.
The second alloy layer was deposited by magnetron sputtering, with the same procedure as in example 1.
Example 10
Embodiment 10 provides a process for forming a metal composite layer on a silver-plated nylon surface, comprising the steps of:
s01: depositing a first silver layer on the surface of the nylon by adopting a chemical silver plating method to obtain the nylon containing the first silver layer;
s02: and depositing a second alloy layer on the surface of the nylon containing the first silver layer by adopting a magnetron sputtering method to obtain the nylon containing the metal composite layer.
The first silver layer is deposited by a chemical silver plating method, and the steps are different from those of the embodiment 1 in that: the total concentration of sodium itaconate in the silver plating reaction liquid in the step (4) is 5 wt%, and sodium tartrate is not contained.
The second alloy layer was deposited by magnetron sputtering, with the same procedure as in example 1.
Example 11
Embodiment 11 provides a process for forming a metal composite layer on a silver-plated nylon surface, comprising the steps of:
s01: depositing a first silver layer on the surface of the nylon by adopting a chemical silver plating method to obtain the nylon containing the first silver layer;
s02: and depositing a second alloy layer on the surface of the nylon containing the first silver layer by adopting a magnetron sputtering method to obtain the nylon containing the metal composite layer.
The first silver layer is deposited by a chemical silver plating method, and the steps are different from those of the embodiment 1 in that: the total concentration of sodium tartrate in the silver plating reaction liquid in the step (4) is 5 wt%, and sodium itaconate is not contained.
The second alloy layer was deposited by magnetron sputtering, with the same procedure as in example 1.
Evaluation of Performance
And (3) flatness evaluation: characterizing the nylon containing the first silver layer prepared in the embodiment by adopting an atomic force microscope, and testing the roughness of the nylon surface; infrared ray reflection performance: the infrared reflectance of the nylon fabrics obtained by the processes of examples 1-5 was greater than 60%.
TABLE 1
Claims (6)
1. A process for forming a metal composite layer on the surface of silver-plated nylon is characterized in that an alloy layer is deposited on the nylon surface containing a silver layer to obtain nylon containing a metal composite layer; the method comprises the following steps:
s01, depositing a first silver layer on the surface of the nylon by adopting a chemical silver plating method to obtain the nylon containing the first silver layer;
s02, depositing a second alloy layer on the nylon surface containing the first silver layer by adopting a magnetron sputtering method to obtain nylon containing a metal composite layer;
the electroless silver plating method in step S01 includes:
(1) washing: cleaning the nylon surface by using water and a detergent to remove oil stains and impurities;
(2) coarsening: placing the cleaned nylon in a chemical coarsening solution, soaking for 10-30min at 20-40 ℃, and then washing with clear water;
(3) sensitization: soaking the cleaned nylon in hydrochloric acid water solution containing stannous chloride at 20-40 deg.c for 10-30min and washing with clear water;
(4) chemical silver plating: placing the sensitized nylon in silver plating reaction liquid, stirring the solution at room temperature for 1min to obtain a mixed solution, then adding sodium tartrate and sodium itaconate into the mixed solution, raising the temperature to 70 ℃, cooling the temperature to room temperature after 30min, then raising the temperature to 70 ℃, repeating the steps of raising the temperature and cooling for three times, and taking out the nylon to obtain the nylon containing the first silver layer;
the molar ratio of the sodium tartrate to the sodium itaconate is 1 (0.6-1.2).
2. The process of claim 1, wherein the second alloy layer is one or more of Ti, Al, Au, In, Ga, Se, La, Ce, Fe, Zn, Cu, W, Mg, Cr, Ni, V, Co, and Pt.
3. The process according to claim 1, wherein the target material assembled in the vacuum sputtering chamber in the magnetron sputtering method in step S02 comprises a metal target material.
4. The process of claim 3, wherein the metal target material comprises a metal titanium target, a metal aluminum target, a metal silver target, a metal zinc target, a metal tin target, an alloy zinc tin target, and an alloy titanium aluminum target.
5. The process according to claim 3, wherein the target material is a planar target, and is connected to a DC power supply, and the sputtering power is 1-40 kW.
6. The process of claim 3, wherein the deposition atmosphere in the vacuum sputtering chamber comprises argon or krypton.
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| JP4844716B2 (en) * | 2005-09-27 | 2011-12-28 | 上村工業株式会社 | Electroless palladium plating bath |
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| CN104032564B (en) * | 2014-06-16 | 2016-01-27 | 东华大学 | A kind of chemical silver plating method of exempting from sensitization activation for polyamide fibre matrix |
| CN208649763U (en) * | 2018-02-05 | 2019-03-26 | 北京纳米生色科技有限公司 | A kind of fabric of the Low emissivity containing the double-deck silver film |
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