CN109881173A - A kind of technique and its product forming metal composite layer on silver coated nylon surface - Google Patents

A kind of technique and its product forming metal composite layer on silver coated nylon surface Download PDF

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Publication number
CN109881173A
CN109881173A CN201910337518.7A CN201910337518A CN109881173A CN 109881173 A CN109881173 A CN 109881173A CN 201910337518 A CN201910337518 A CN 201910337518A CN 109881173 A CN109881173 A CN 109881173A
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layer
nylon
silver
target
metal composite
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CN109881173B (en
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商承杰
商蔚
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Beijing Jlsun High-Tech Co Ltd
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Beijing Jlsun High-Tech Co Ltd
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Abstract

The present invention relates to nylon processing technique fields, and in particular to a kind of technique and its product for forming metal composite layer on silver coated nylon surface.A kind of technique forming metal composite layer on silver coated nylon surface includes the following steps: to obtain the nylon containing metal composite layer in the nylon surface deposit alloy layer of Ag containing layer using magnetically controlled sputter method.The flatness on the nylon surface that the present invention is prepared is preferable, have the function of to the processed and applied of the nylon in later period positive, and there is preferable infra-red radiation barrier property using nylon product made from the technique, play the role of heat-insulation warm keeping, it is used in space shuttle and guided missile etc., it is not only light, high-strength, non-discolouring and durable, but also additionally provide the novel silver-plated antenna space material of one kind and flexible electrode material.It is used in textile, fabric can not only be made to have the effect of cool in summer and warm in winter, will not also reduce the visibility of fabric color and texture, so that the color of fabric and texture be made to show preferable effect.

Description

A kind of technique and its product forming metal composite layer on silver coated nylon surface
Technical field
The invention belongs to nylon processing technique fields, more particularly it relates to which a kind of form on silver coated nylon surface The technique and its product of metal composite layer.
Background technique
Object is under the prolonged exposure of sunlight, especially in the hot summer, can gather amount of heat, leads to its internal temperature Degree increases, and brings inconvenience and harm to people's production and life.As the improvement of people's living standards, outdoor activities It is becoming increasingly popular, current outdoor textile does not obstruct the infra-red radiation that solar energy 46% is accounted in sunlight well Effect needs a kind of open air with infrared external reflection function to reduce hot environment to people's production, life bring trouble Textile.A kind of film layer that can reflect infrared ray is plated on nylon surface, in hot environment, sun sending can be obstructed Infra-red radiation, while the infrared radiation loss of covering in nylon can be reduced in cold winter, to meet heat-insulation and heat-preservation Demand.Will be new as a kind of heat-insulation warm keeping that can be widely used using outdoor textile made by this nylon Solution.
Metallic silver has the function of extraordinary infrared external reflection, and the thickness of film layer is bigger, gets over to the reflecting effect of infrared ray It is good.But silver film is easy to oxidize in coating process, and flatness is caused to reduce, so that the uneven thickness of nylon surface silver film One, and the exponential transmission for reducing visible light of the excessively high meeting of thickness, so that the color of fabric and texture visibility be made to reduce, therefore give People bring faulty using effect.
Summary of the invention
To solve the above-mentioned problems, the present invention provides it is a kind of silver coated nylon surface formed metal composite layer technique, Include the following steps: the nylon surface deposit alloy layer in Ag containing layer, obtains the nylon containing metal composite layer.
As a kind of perferred technical scheme, the nylon containing metal composite layer uses vacuum evaporation technology or metal It is organic chemical vapor deposition method, pulsed laser deposition, spray heating decomposition, molecular beam epitaxy, plasma spray coating, more One of arc ion vacuum coating technique, optical vacuum coating technique, other vacuum coatings, chemical silvering or multiple technologies shape At.
As a kind of perferred technical scheme, include the following steps:
S01: the first silver layer is deposited on nylon surface using chemical silver plating method, obtains the nylon containing the first silver layer;
S02: the second alloy-layer is deposited on the nylon surface containing the first silver layer using magnetically controlled sputter method, is obtained multiple containing metal Close the nylon of layer.
As a kind of perferred technical scheme, second alloy-layer be by Ti, Al, Au, In, Ga, Se, La, Ce, Fe, One or more of Zn, Cu, W, Mg, Cr, Ni, V, Co, Pt element composition.
As a kind of perferred technical scheme, second alloy-layer is AZO (ZnO:Al2O3) transparent conductive film layer.
As a kind of perferred technical scheme, second alloy-layer is ito thin film layer.
As a kind of perferred technical scheme, assembly in vacuum sputtering cavity in magnetically controlled sputter method in the step S02 Target include metal targets and ceramic target.
As a kind of perferred technical scheme, the metal targets include metal titanium targets, metallic aluminium target, metallic silver target, gold Belong to zinc target, metal tin target, alloy zinc-tin target, titanium alloy aluminium target;The ceramic target include titanium oxide ceramics target, sial target, AZO ceramic target, iron oxide ceramics target, ITO ceramic target.
As a kind of perferred technical scheme, the target is flat target, meets DC power supply, sputtering power 1-40kW.
As a kind of perferred technical scheme, the intracorporal deposition atmosphere of vacuum sputtering chamber includes argon gas, Krypton.
The utility model has the advantages that, processing to the nylon in later period preferable using the flatness on the nylon surface of the invention being prepared It is positive using having the function of, and there is preferable infra-red radiation barrier property using nylon product made from the technique, it plays The effect of heat-insulation warm keeping, and application is relatively broad, uses in textile, and fabric can not only be made to have effect cool in summer and warm in winter Fruit, will not also reduce the visibility of fabric color and texture, so that the color of fabric and texture be made to show preferable effect.
Specific embodiment
It is further clear, complete that the technical characteristic work in technical solution is provided to the present invention With reference to embodiment Description, not to the limitation of its protection scope.
Word " preferred ", " preferred " in the present invention etc. refer to, can provide in some cases certain beneficial to effect The embodiment of the present invention of fruit.However, other embodiments are also likely to be preferred under identical circumstances or in the case of other 's.In addition, do not imply that other embodiments are unavailable to the statement of one or more preferred embodiments, be also not intended to by Other embodiments exclude except the scope of the present invention.
To solve the above-mentioned problems, the present invention provides it is a kind of silver coated nylon surface formed metal composite layer technique, Include the following steps: the nylon surface deposit alloy layer in Ag containing layer, obtains the nylon containing metal composite layer.
In a preferred embodiment, the nylon containing metal composite layer uses vacuum evaporation technology or metal It is organic chemical vapor deposition method, pulsed laser deposition, spray heating decomposition, molecular beam epitaxy, plasma spray coating, more One of arc ion vacuum coating technique, optical vacuum coating technique, other vacuum coatings, chemical silvering or multiple technologies shape At.
As a kind of perferred technical scheme, include the following steps:
S01: the first silver layer is deposited on nylon surface using chemical silver plating method, obtains the nylon containing the first silver layer;
S02: the second alloy-layer is deposited on the nylon surface containing the first silver layer using magnetically controlled sputter method, is obtained multiple containing metal Close the nylon of layer.
First silver layer
In some embodiments, chemical silver plating method includes: in step S01 of the present invention
(1) it washs: nylon surface being cleaned with water and detergent, degrease and impurity;
(2) it is roughened: the nylon of above-mentioned washes clean is placed in chemical coarsening solution, impregnates 10-30min at 20-40 DEG C It is washed afterwards with clear water;
(3) it is sensitized: the nylon of above-mentioned washes clean being placed in the aqueous hydrochloric acid solution of chloride containing stannous, at 20-40 DEG C It is washed after impregnating 10-30min with clear water;
(4) chemical silvering: the nylon after above-mentioned sensitization is placed in silver plating reaction liquid, and 1min is stirred at room temperature in solution and is obtained Sodium tartrate and sodium itaconate is added in mixed solution thereto later, increases temperature to 70 DEG C, room is cooled the temperature to after 30min Temperature increases temperature to 70 DEG C again later, repeats to heat up cooling step three times, takes out nylon and obtain the Buddhist nun containing the first silver layer Dragon.
In a preferred embodiment, in step (2) of the present invention: the concentration of nylon is in chemical coarsening solution 20wt%, it is described chemistry coarsening solution be containing ascorbic acid, sodium hydroxide, cetyl trimethylammonium bromide, water mixed solution, The ascorbic acid, sodium hydroxide, cetyl trimethylammonium bromide, water mass ratio be (0.01-0.06): (0.02- 0.08): (0.02-0.1): 1, it is furthermore preferred that the matter of the ascorbic acid, sodium hydroxide, cetyl trimethylammonium bromide, water Amount is than being 0.05:0.06:0.05:1.
In a preferred embodiment, in step (3) of the present invention: Buddhist nun in the aqueous hydrochloric acid solution of chloride containing stannous The concentration of dragon is 30wt%, stannous chloride in the aqueous hydrochloric acid solution of the chloride containing stannous, concentrated hydrochloric acid, water mass ratio be (0.02-0.05): (0.02-0.06): 1, it is furthermore preferred that the mass ratio of the stannous chloride, concentrated hydrochloric acid, water is 0.03:0.04: 1。
In a preferred embodiment, in step (4) of the present invention: silver plating reaction liquid be containing silver nitrate, ammonium hydroxide, The mixed solution of potassium hydroxide, ethyl alcohol, the silver nitrate, ammonium hydroxide, potassium hydroxide, ethyl alcohol mass ratio be (0.2-0.5): (0.4-0.8): (0.05-0.1): 1, it is furthermore preferred that the mass ratio of the silver nitrate, ammonium hydroxide, potassium hydroxide, ethyl alcohol is 0.3: 0.6:0.06:1.
In a preferred embodiment, in step (4) of the present invention: the concentration of nylon is in silver plating reaction liquid The total concentration of 25wt%, the silver plating reaction liquid mesotartaric acid sodium and sodium itaconate is 2wt%-10wt%, the sodium tartrate Molar ratio with sodium itaconate is 1:(0.6-1.2);It is furthermore preferred that the silver plating reaction liquid mesotartaric acid sodium and sodium itaconate Total concentration is 5wt%, and the molar ratio of the sodium tartrate and sodium itaconate is 1:1.
The applicant is found surprisingly that when preparing the nylon containing the first silver layer, and sodium tartrate and sodium itaconate is added Afterwards, the silverskin flatness of deposition is higher.Inventor speculates the possible reason is the addition of the two facilitates the reduction of silver, as crystalline substance Core, while four carbon on sodium tartrate can form four points of crystal growth, be conducive to the rapid growth of silver.Meanwhile Under the collaboration of sodium itaconate, under concave region, the extra convex domain of point of sodium tartrate, so that the growth of silver more has selection Property.In addition, inventor also found when the molar ratio of sodium tartrate and sodium itaconate is 1:(0.6-1.2) when, to above-mentioned effect Better effect, inventor's supposition may be that four carbon on sodium tartrate can form four points that crystal increases, sodium itaconate There are two hydroxyls to have certain chelation for upper tool, accelerates the molding of silver.
Second alloy-layer
In a preferred embodiment, the second alloy-layer of the present invention is deposited by magnetically controlled sputter method.
Magnetron sputtering method of the present invention is to be filled with suitable argon gas in high vacuum, in cathode (Style Columu Talget or flat target) and Apply several hundred K DC voltages between anode (plated film locular wall), magnet controlled abnormal glow discharge is generated in coating chamber, sends out argon gas Raw ionization;Argon ion accelerates simultaneously bombarding cathode target surface by cathode, and target material surface atom sputtering is come out and is deposited on substrate surface Upper formation film.
In some embodiments, second alloy-layer be by Ti, Al, Au, In, Ga, Se, La, Ce, Fe, Zn, Cu, W, one or more of Mg, Cr, Ni, V, Co, Pt element form.
In some embodiments, the target of assembly includes in vacuum sputtering cavity in magnetically controlled sputter method of the present invention Metal targets;Wherein, the metal targets include metal titanium targets, metallic aluminium target, metallic silver target, metallic zinc target, metal tin target, conjunction Golden zinc-tin target, titanium alloy aluminium target.
In some embodiments, the intracorporal deposition atmosphere of vacuum sputtering chamber of the present invention includes argon gas, Krypton.
In some embodiments, the intracorporal target of vacuum sputtering chamber of the present invention is flat target, connects DC power supply, splashes Penetrating power is 1-40kW.
In some embodiments, the second alloy-layer of the present invention is deposited by magnetically controlled sputter method, and step includes: The above-mentioned nylon for containing the first silver layer is placed in continuous vacuum sputtering cavity and carries out magnetron sputtering film forming, in sputter chamber deposition the Two alloy-layers, target are any one of titanium alloy aluminium target, ITO ceramic target, AZO ceramic target, and atmosphere is pure argon, and air pressure is 0.5-1Pa, DC power supply sputtering power 7-12kW, control the second alloy-layer with a thickness of 1-15nm, obtain containing metal composite The nylon of layer.
In a preferred embodiment, the second alloy-layer of the present invention is titanium-aluminium alloy layer.
In a preferred embodiment, the second alloy-layer of the present invention is deposited by magnetically controlled sputter method, step It suddenly include: that the nylon containing the first silver layer is placed in continuous vacuum sputtering cavity to carry out magnetron sputtering film forming, it is heavy in sputter chamber The second alloy-layer of product, target are titanium alloy aluminium target, and atmosphere is pure argon, air pressure 0.5Pa, DC power supply sputtering power 9kW, control Make the second alloy-layer with a thickness of 8nm, obtain the nylon containing metal composite layer.
In a preferred embodiment, the second alloy-layer of the present invention is AZO (ZnO:Al2O3) electrically conducting transparent is thin Film layer.
In a preferred embodiment, the second alloy-layer of the present invention is deposited by magnetically controlled sputter method, step It suddenly include: that the nylon containing the first silver layer is placed in continuous vacuum sputtering cavity to carry out magnetron sputtering film forming, it is heavy in sputter chamber The second alloy-layer of product, target are AZO ceramic target, and atmosphere is pure argon, air pressure 0.5Pa, DC power supply sputtering power 9kW, control Make the second alloy-layer with a thickness of 8nm, obtain the nylon containing metal composite layer.
In a preferred embodiment, the second alloy-layer of the present invention is ito thin film layer.
In a preferred embodiment, the second alloy-layer of the present invention is deposited by magnetically controlled sputter method, step It suddenly include: that the nylon containing the first silver layer is placed in continuous vacuum sputtering cavity to carry out magnetron sputtering film forming, it is heavy in sputter chamber The second alloy-layer of product, target are ITO ceramic target, and atmosphere is pure argon, air pressure 0.5Pa, DC power supply sputtering power 9kW, control Make the second alloy-layer with a thickness of 8nm, obtain the nylon containing metal composite layer.
The second aspect of the present invention provides a kind of nylon containing metal composite layer in fabric, non-woven fabrics, artificial leather, sea Silk floss, plastic film, flexible material, clothes, the application on bed necessaries.
The present invention is specifically described below by embodiment, in addition, if without other explanations, it is raw materials used to be all It is commercially available.
Embodiment
Embodiment 1
Embodiment 1 provides a kind of technique that metal composite layer is formed on silver coated nylon surface, includes the following steps:
S01: the first silver layer is deposited on nylon surface using chemical silver plating method, obtains the nylon containing the first silver layer;
S02: the second alloy-layer is deposited on the nylon surface containing the first silver layer using magnetically controlled sputter method, is obtained multiple containing metal Close the nylon of layer.
First silver layer is deposited by chemical silver plating method, and step includes:
(1) it washs: nylon surface being cleaned with water and detergent, degrease and impurity;
(2) it is roughened: the nylon of above-mentioned washes clean is placed in chemical coarsening solution, impregnates 10-30min at 20-40 DEG C It is washed afterwards with clear water;
(3) it is sensitized: the nylon of above-mentioned washes clean being placed in the aqueous hydrochloric acid solution of chloride containing stannous, at 20-40 DEG C It is washed after impregnating 10-30min with clear water;
(4) chemical silvering: the nylon after above-mentioned sensitization is placed in silver plating reaction liquid, and 1min is stirred at room temperature in solution and is obtained Sodium tartrate and sodium itaconate is added in mixed solution thereto later, increases temperature to 70 DEG C, room is cooled the temperature to after 30min Temperature increases temperature to 70 DEG C again later, repeats to heat up cooling step three times, takes out nylon and obtain the Buddhist nun containing the first silver layer Dragon.
Wherein, in the step (2): in chemical coarsening solution the concentration of nylon be 20wt%, it is described chemistry coarsening solution be containing Ascorbic acid, sodium hydroxide, cetyl trimethylammonium bromide, water mixed solution, the ascorbic acid, sodium hydroxide, ten Six alkyl trimethyl ammonium bromides, water mass ratio be 0.05:0.06:0.05:1.
In the step (3): the concentration of nylon is 30wt%, the protochloride in the aqueous hydrochloric acid solution of chloride containing stannous Tin, concentrated hydrochloric acid, water mass ratio be 0.03:0.04:1.
In the step (4): silver plating reaction liquid be containing silver nitrate, ammonium hydroxide, potassium hydroxide, ethyl alcohol mixed solution, it is described Silver nitrate, ammonium hydroxide, potassium hydroxide, ethyl alcohol mass ratio be 0.3:0.6:0.06:1;The concentration of nylon is in silver plating reaction liquid The total concentration of 25wt%, the silver plating reaction liquid mesotartaric acid sodium and sodium itaconate is 5wt%, the sodium tartrate and itaconic acid The molar ratio of sodium is 1:1.
Second alloy-layer is deposited by magnetically controlled sputter method, and step includes: by the above-mentioned nylon for containing the first silver layer It is placed in continuous vacuum sputtering cavity and carries out magnetron sputtering film forming, deposit the second alloy-layer in sputter chamber, target is titanium alloy Aluminium target, atmosphere are pure argon, air pressure 0.5Pa, DC power supply sputtering power 9kW, the second alloy-layer of control with a thickness of 8nm, Obtain the nylon containing metal composite layer.
Embodiment 2
Embodiment 2 provides a kind of technique that metal composite layer is formed on silver coated nylon surface, includes the following steps:
S01: the first silver layer is deposited on nylon surface using chemical silver plating method, obtains the nylon containing the first silver layer;
S02: the second alloy-layer is deposited on the nylon surface containing the first silver layer using magnetically controlled sputter method, is obtained multiple containing metal Close the nylon of layer.
First silver layer is deposited by chemical silver plating method, and step includes:
(1) it washs: nylon surface being cleaned with water and detergent, degrease and impurity;
(2) it is roughened: the nylon of above-mentioned washes clean is placed in chemical coarsening solution, impregnates 10-30min at 20-40 DEG C It is washed afterwards with clear water;
(3) it is sensitized: the nylon of above-mentioned washes clean being placed in the aqueous hydrochloric acid solution of chloride containing stannous, at 20-40 DEG C It is washed after impregnating 10-30min with clear water;
(4) chemical silvering: the nylon after above-mentioned sensitization is placed in silver plating reaction liquid, and 1min is stirred at room temperature in solution and is obtained Sodium tartrate and sodium itaconate is added in mixed solution thereto later, increases temperature to 70 DEG C, room is cooled the temperature to after 30min Temperature increases temperature to 70 DEG C again later, repeats to heat up cooling step three times, takes out nylon and obtain the Buddhist nun containing the first silver layer Dragon.
Wherein, in the step (2): in chemical coarsening solution the concentration of nylon be 20wt%, it is described chemistry coarsening solution be containing Ascorbic acid, sodium hydroxide, cetyl trimethylammonium bromide, water mixed solution, the ascorbic acid, sodium hydroxide, ten Six alkyl trimethyl ammonium bromides, water mass ratio be 0.05:0.06:0.05:1.
In the step (3): the concentration of nylon is 30wt%, the protochloride in the aqueous hydrochloric acid solution of chloride containing stannous Tin, concentrated hydrochloric acid, water mass ratio be 0.03:0.04:1.
In the step (4): silver plating reaction liquid be containing silver nitrate, ammonium hydroxide, potassium hydroxide, ethyl alcohol mixed solution, it is described Silver nitrate, ammonium hydroxide, potassium hydroxide, ethyl alcohol mass ratio be 0.3:0.6:0.06:1;The concentration of nylon is in silver plating reaction liquid The total concentration of 25wt%, the silver plating reaction liquid mesotartaric acid sodium and sodium itaconate is 2wt%, the sodium tartrate and itaconic acid The molar ratio of sodium is 1:0.6.
Second alloy-layer is deposited by magnetically controlled sputter method, and step includes: to be placed in the nylon containing the first silver layer Continuous vacuum sputtering cavity carries out magnetron sputtering film forming, deposits the second alloy-layer in sputter chamber, and target is AZO ceramic target, Atmosphere is pure argon, air pressure 0.5Pa, DC power supply sputtering power 9kW, the second alloy-layer of control with a thickness of 8nm, contained There is the nylon of metal composite layer.
Embodiment 3
Embodiment 3 provides a kind of technique that metal composite layer is formed on silver coated nylon surface, includes the following steps:
S01: the first silver layer is deposited on nylon surface using chemical silver plating method, obtains the nylon containing the first silver layer;
S02: the second alloy-layer is deposited on the nylon surface containing the first silver layer using magnetically controlled sputter method, is obtained multiple containing metal Close the nylon of layer.
First silver layer is deposited by chemical silver plating method, and step includes:
(1) it washs: nylon surface being cleaned with water and detergent, degrease and impurity;
(2) it is roughened: the nylon of above-mentioned washes clean is placed in chemical coarsening solution, impregnates 10-30min at 20-40 DEG C It is washed afterwards with clear water;
(3) it is sensitized: the nylon of above-mentioned washes clean being placed in the aqueous hydrochloric acid solution of chloride containing stannous, at 20-40 DEG C It is washed after impregnating 10-30min with clear water;
(4) chemical silvering: the nylon after above-mentioned sensitization is placed in silver plating reaction liquid, and 1min is stirred at room temperature in solution and is obtained Sodium tartrate and sodium itaconate is added in mixed solution thereto later, increases temperature to 70 DEG C, room is cooled the temperature to after 30min Temperature increases temperature to 70 DEG C again later, repeats to heat up cooling step three times, takes out nylon and obtain the Buddhist nun containing the first silver layer Dragon.
Wherein, in the step (2): in chemical coarsening solution the concentration of nylon be 20wt%, it is described chemistry coarsening solution be containing Ascorbic acid, sodium hydroxide, cetyl trimethylammonium bromide, water mixed solution, the ascorbic acid, sodium hydroxide, ten Six alkyl trimethyl ammonium bromides, water mass ratio be 0.05:0.06:0.05:1.
In the step (3): the concentration of nylon is 30wt%, the protochloride in the aqueous hydrochloric acid solution of chloride containing stannous Tin, concentrated hydrochloric acid, water mass ratio be 0.03:0.04:1.
In the step (4): silver plating reaction liquid be containing silver nitrate, ammonium hydroxide, potassium hydroxide, ethyl alcohol mixed solution, it is described Silver nitrate, ammonium hydroxide, potassium hydroxide, ethyl alcohol mass ratio be 0.3:0.6:0.06:1;The concentration of nylon is in silver plating reaction liquid The total concentration of 25wt%, the silver plating reaction liquid mesotartaric acid sodium and sodium itaconate is 10wt%, the sodium tartrate and clothing health The molar ratio of sour sodium is 1:1.2.
Second alloy-layer is deposited by magnetically controlled sputter method, and step includes: to be placed in the nylon containing the first silver layer Continuous vacuum sputtering cavity carries out magnetron sputtering film forming, deposits the second alloy-layer in sputter chamber, and target is ITO ceramic target, Atmosphere is pure argon, air pressure 0.5Pa, DC power supply sputtering power 9kW, the second alloy-layer of control with a thickness of 8nm, contained There is the nylon of metal composite layer.
Embodiment 4
Embodiment 4 provides a kind of technique that metal composite layer is formed on silver coated nylon surface, includes the following steps:
S01: the first silver layer is deposited on nylon surface using chemical silver plating method, obtains the nylon containing the first silver layer;
S02: the second alloy-layer is deposited on the nylon surface containing the first silver layer using magnetically controlled sputter method, is obtained multiple containing metal Close the nylon of layer.
First silver layer is deposited by chemical silver plating method, and step includes:
(1) it washs: nylon surface being cleaned with water and detergent, degrease and impurity;
(2) it is roughened: the nylon of above-mentioned washes clean is placed in chemical coarsening solution, impregnates 10-30min at 20-40 DEG C It is washed afterwards with clear water;
(3) it is sensitized: the nylon of above-mentioned washes clean being placed in the aqueous hydrochloric acid solution of chloride containing stannous, at 20-40 DEG C It is washed after impregnating 10-30min with clear water;
(4) chemical silvering: the nylon after above-mentioned sensitization is placed in silver plating reaction liquid, and 1min is stirred at room temperature in solution and is obtained Sodium tartrate and sodium itaconate is added in mixed solution thereto later, increases temperature to 70 DEG C, room is cooled the temperature to after 30min Temperature increases temperature to 70 DEG C again later, repeats to heat up cooling step three times, takes out nylon and obtain the Buddhist nun containing the first silver layer Dragon.
Wherein, in the step (2): in chemical coarsening solution the concentration of nylon be 20wt%, it is described chemistry coarsening solution be containing Ascorbic acid, sodium hydroxide, cetyl trimethylammonium bromide, water mixed solution, the ascorbic acid, sodium hydroxide, ten Six alkyl trimethyl ammonium bromides, water mass ratio be 0.05:0.06:0.05:1.
In the step (3): the concentration of nylon is 30wt%, the protochloride in the aqueous hydrochloric acid solution of chloride containing stannous Tin, concentrated hydrochloric acid, water mass ratio be 0.03:0.04:1.
In the step (4): silver plating reaction liquid be containing silver nitrate, ammonium hydroxide, potassium hydroxide, ethyl alcohol mixed solution, it is described Silver nitrate, ammonium hydroxide, potassium hydroxide, ethyl alcohol mass ratio be 0.3:0.6:0.06:1;The concentration of nylon is in silver plating reaction liquid The total concentration of 25wt%, the silver plating reaction liquid mesotartaric acid sodium and sodium itaconate is 3wt%, the sodium tartrate and itaconic acid The molar ratio of sodium is 1:0.8.
Second alloy-layer is deposited by magnetically controlled sputter method, and step includes: by the above-mentioned nylon for containing the first silver layer It is placed in continuous vacuum sputtering cavity and carries out magnetron sputtering film forming, deposit the second alloy-layer in sputter chamber, target is titanium alloy Aluminium target, atmosphere are pure argon, air pressure 0.5Pa, DC power supply sputtering power 9kW, the second alloy-layer of control with a thickness of 8nm, Obtain the nylon containing metal composite layer.
Embodiment 5
Embodiment 5 provides a kind of technique that metal composite layer is formed on silver coated nylon surface, includes the following steps:
S01: the first silver layer is deposited on nylon surface using chemical silver plating method, obtains the nylon containing the first silver layer;
S02: the second alloy-layer is deposited on the nylon surface containing the first silver layer using magnetically controlled sputter method, is obtained multiple containing metal Close the nylon of layer.
First silver layer is deposited by chemical silver plating method, and step includes:
(1) it washs: nylon surface being cleaned with water and detergent, degrease and impurity;
(2) it is roughened: the nylon of above-mentioned washes clean is placed in chemical coarsening solution, impregnates 10-30min at 20-40 DEG C It is washed afterwards with clear water;
(3) it is sensitized: the nylon of above-mentioned washes clean being placed in the aqueous hydrochloric acid solution of chloride containing stannous, at 20-40 DEG C It is washed after impregnating 10-30min with clear water;
(4) chemical silvering: the nylon after above-mentioned sensitization is placed in silver plating reaction liquid, and 1min is stirred at room temperature in solution and is obtained Sodium tartrate and sodium itaconate is added in mixed solution thereto later, increases temperature to 70 DEG C, room is cooled the temperature to after 30min Temperature increases temperature to 70 DEG C again later, repeats to heat up cooling step three times, takes out nylon and obtain the Buddhist nun containing the first silver layer Dragon.
Wherein, in the step (2): in chemical coarsening solution the concentration of nylon be 20wt%, it is described chemistry coarsening solution be containing Ascorbic acid, sodium hydroxide, cetyl trimethylammonium bromide, water mixed solution, the ascorbic acid, sodium hydroxide, ten Six alkyl trimethyl ammonium bromides, water mass ratio be 0.05:0.06:0.05:1.
In the step (3): the concentration of nylon is 30wt%, the protochloride in the aqueous hydrochloric acid solution of chloride containing stannous Tin, concentrated hydrochloric acid, water mass ratio be 0.03:0.04:1.
In the step (4): silver plating reaction liquid be containing silver nitrate, ammonium hydroxide, potassium hydroxide, ethyl alcohol mixed solution, it is described Silver nitrate, ammonium hydroxide, potassium hydroxide, ethyl alcohol mass ratio be 0.3:0.6:0.06:1;The concentration of nylon is in silver plating reaction liquid The total concentration of 25wt%, the silver plating reaction liquid mesotartaric acid sodium and sodium itaconate is 7wt%, the sodium tartrate and itaconic acid The molar ratio of sodium is 1:1.
Second alloy-layer is deposited by magnetically controlled sputter method, and step includes: by the above-mentioned nylon for containing the first silver layer It is placed in continuous vacuum sputtering cavity and carries out magnetron sputtering film forming, deposit the second alloy-layer in sputter chamber, target is titanium alloy Aluminium target, atmosphere are pure argon, air pressure 0.5Pa, DC power supply sputtering power 9kW, the second alloy-layer of control with a thickness of 8nm, Obtain the nylon containing metal composite layer.
Embodiment 6
Embodiment 6 provides a kind of technique that metal composite layer is formed on silver coated nylon surface, includes the following steps:
S01: the first silver layer is deposited on nylon surface using chemical silver plating method, obtains the nylon containing the first silver layer;
S02: the second alloy-layer is deposited on the nylon surface containing the first silver layer using magnetically controlled sputter method, is obtained multiple containing metal Close the nylon of layer.
First silver layer is deposited by chemical silver plating method, and step difference from Example 1 is: step (4) Described in the total concentration of silver plating reaction liquid mesotartaric acid sodium and sodium itaconate be 0wt%.
Second alloy-layer is deposited by magnetically controlled sputter method, and step is the same as embodiment 1.
Embodiment 7
Embodiment 7 provides a kind of technique that metal composite layer is formed on silver coated nylon surface, includes the following steps:
S01: the first silver layer is deposited on nylon surface using chemical silver plating method, obtains the nylon containing the first silver layer;
S02: the second alloy-layer is deposited on the nylon surface containing the first silver layer using magnetically controlled sputter method, is obtained multiple containing metal Close the nylon of layer.
First silver layer is deposited by chemical silver plating method, and step difference from Example 1 is: step (4) Described in the total concentration of silver plating reaction liquid mesotartaric acid sodium and sodium itaconate be 30wt%.
Second alloy-layer is deposited by magnetically controlled sputter method, and step is the same as embodiment 1.
Embodiment 8
Embodiment 8 provides a kind of technique that metal composite layer is formed on silver coated nylon surface, includes the following steps:
S01: the first silver layer is deposited on nylon surface using chemical silver plating method, obtains the nylon containing the first silver layer;
S02: the second alloy-layer is deposited on the nylon surface containing the first silver layer using magnetically controlled sputter method, is obtained multiple containing metal Close the nylon of layer.
First silver layer is deposited by chemical silver plating method, and step difference from Example 1 is: step (4) Described in the total concentration of silver plating reaction liquid mesotartaric acid sodium and sodium itaconate be 5wt%, the sodium tartrate and sodium itaconate Molar ratio is 1:0.1.
Second alloy-layer is deposited by magnetically controlled sputter method, and step is the same as embodiment 1.
Embodiment 9
Embodiment 9 provides a kind of technique that metal composite layer is formed on silver coated nylon surface, includes the following steps:
S01: the first silver layer is deposited on nylon surface using chemical silver plating method, obtains the nylon containing the first silver layer;
S02: the second alloy-layer is deposited on the nylon surface containing the first silver layer using magnetically controlled sputter method, is obtained multiple containing metal Close the nylon of layer.
First silver layer is deposited by chemical silver plating method, and step difference from Example 1 is: step (4) Described in the total concentration of silver plating reaction liquid mesotartaric acid sodium and sodium itaconate be 5wt%, the sodium tartrate and sodium itaconate Molar ratio is 1:22.
Second alloy-layer is deposited by magnetically controlled sputter method, and step is the same as embodiment 1.
Embodiment 10
Embodiment 10 provides a kind of technique that metal composite layer is formed on silver coated nylon surface, includes the following steps:
S01: the first silver layer is deposited on nylon surface using chemical silver plating method, obtains the nylon containing the first silver layer;
S02: the second alloy-layer is deposited on the nylon surface containing the first silver layer using magnetically controlled sputter method, is obtained multiple containing metal Close the nylon of layer.
First silver layer is deposited by chemical silver plating method, and step difference from Example 1 is: step (4) Described in silver plating reaction liquid the total concentration of sodium itaconate be 5wt%, be free of sodium tartrate.
Second alloy-layer is deposited by magnetically controlled sputter method, and step is the same as embodiment 1.
Embodiment 11
Embodiment 11 provides a kind of technique that metal composite layer is formed on silver coated nylon surface, includes the following steps:
S01: the first silver layer is deposited on nylon surface using chemical silver plating method, obtains the nylon containing the first silver layer;
S02: the second alloy-layer is deposited on the nylon surface containing the first silver layer using magnetically controlled sputter method, is obtained multiple containing metal Close the nylon of layer.
First silver layer is deposited by chemical silver plating method, and step difference from Example 1 is: step (4) Described in silver plating reaction liquid mesotartaric acid sodium total concentration be 5wt%, be free of sodium itaconate.
Second alloy-layer is deposited by magnetically controlled sputter method, and step is the same as embodiment 1.
Performance evaluation
Flatness evaluation: the preparation-obtained nylon for containing the first silver layer of embodiment is used into atomic force microscope carry out table Sign tests the roughness on nylon surface;Reflection infrared linear energy: the nylon fabric obtained using the technique of embodiment 1-5 it is red Outside line reflectivity is all larger than 60%.
Table 1

Claims (10)

1. a kind of technique for forming metal composite layer on silver coated nylon surface, which comprises the steps of: in Ag containing layer Nylon surface deposit alloy layer, obtain the nylon containing metal composite layer.
2. the technique according to claim 1 for forming metal composite layer on silver coated nylon surface, which is characterized in that described to contain The nylon of metal composite layer uses vacuum evaporation technology or metal-organic chemical vapor deposition equipment method, pulsed laser deposition, spray Mist thermal decomposition method, molecular beam epitaxy, plasma spray coating, multi sphere ion vacuum coating technique, optical vacuum coating technique, its One of his vacuum coating, chemical silvering or multiple technologies are formed.
3. the technique according to claim 1 for forming metal composite layer on silver coated nylon surface, which is characterized in that including such as Lower step:
S01: the first silver layer is deposited on nylon surface using chemical silver plating method, obtains the nylon containing the first silver layer;
S02: the second alloy-layer is deposited on the nylon surface containing the first silver layer using magnetically controlled sputter method, is obtained containing metal composite layer Nylon.
4. the technique according to claim 3 for forming metal composite layer on silver coated nylon surface, which is characterized in that described the Two alloy-layers are by one or more of Ti, Al, Au, In, Ga, Se, La, Ce, Fe, Zn, Cu, W, Mg, Cr, Ni, V, Co, Pt Element composition.
5. the technique according to claim 3 for forming metal composite layer on silver coated nylon surface, which is characterized in that described the Two alloy-layers are AZO (ZnO:Al2O3) transparent conductive film layer.
6. the technique according to claim 3 for forming metal composite layer on silver coated nylon surface, which is characterized in that described the Two alloy-layers are ito thin film layers.
7. the technique according to claim 3 for forming metal composite layer on silver coated nylon surface, which is characterized in that the step The target assembled in vacuum sputtering cavity in magnetically controlled sputter method in rapid S02 includes metal targets and ceramic target.
8. the technique according to claim 7 for forming metal composite layer on silver coated nylon surface, which is characterized in that the gold Belonging to target includes metal titanium targets, metallic aluminium target, metallic silver target, metallic zinc target, metal tin target, alloy zinc-tin target, titanium alloy aluminium target; The ceramic target includes titanium oxide ceramics target, sial target, AZO ceramic target, iron oxide ceramics target, ITO ceramic target.
9. the technique according to claim 7 for forming metal composite layer on silver coated nylon surface, which is characterized in that the target Material is flat target, meets DC power supply, sputtering power 1-40kW.
10. the technique according to claim 7 for forming metal composite layer on silver coated nylon surface, which is characterized in that described The intracorporal deposition atmosphere of vacuum sputtering chamber includes argon gas, Krypton.
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CN102758352A (en) * 2011-04-27 2012-10-31 苏州市奥普斯等离子体科技有限公司 Fabric surface metallization processing method
CN104032564A (en) * 2014-06-16 2014-09-10 东华大学 Sensitization-free and activation-free chemical silvering method for polyamide base body
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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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006030254A1 (en) * 2004-09-15 2006-03-23 Kabushiki Kaisha Suzutora (Suzutora Corporation) Metal-coated textile
CN1687507A (en) * 2005-04-12 2005-10-26 夏芝林 Method for preparing silver metallized organic fiber and textile
CN101356299A (en) * 2005-09-27 2009-01-28 上村工业株式会社 Electroless palladium plating bath and electroless palladium plating method
CN102758352A (en) * 2011-04-27 2012-10-31 苏州市奥普斯等离子体科技有限公司 Fabric surface metallization processing method
CN104032564A (en) * 2014-06-16 2014-09-10 东华大学 Sensitization-free and activation-free chemical silvering method for polyamide base body
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