CN114032507B - Double-sided vacuum aluminum film plating process - Google Patents

Double-sided vacuum aluminum film plating process Download PDF

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Publication number
CN114032507B
CN114032507B CN202111391325.3A CN202111391325A CN114032507B CN 114032507 B CN114032507 B CN 114032507B CN 202111391325 A CN202111391325 A CN 202111391325A CN 114032507 B CN114032507 B CN 114032507B
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sided
double
vacuum
aluminizer
aluminum
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CN114032507A (en
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林善华
陈永群
魏国华
张航
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Foshan Cailong Coating Packaging Materials Co ltd
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Foshan Cailong Coating Packaging Materials Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/20—Metallic material, boron or silicon on organic substrates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • C23C14/562—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks for coating elongated substrates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment

Abstract

The application relates to the technical field of vacuum aluminizing films, and particularly discloses a double-sided vacuum aluminizing film process, which comprises the following preparation steps: step one, preparing an aluminum material; step two, preparing a composite glue solution, coating the composite glue solution on a substrate, and then heating and carrying out irradiation treatment at the same time until the moisture is evaporated to dryness to prepare a base film; step three, vacuum evaporation for one time: the thickness of the plating layer is 800-1000 angstroms to obtain a single-side aluminizer; placing the single-sided aluminizer on an aluminizing drum and rewinding for one time; step five, secondary vacuum evaporation: the thickness of the plating layer is 500-600 angstroms to obtain a double-sided aluminum plating film; step six, thinning the double-sided aluminizer: uniformly cooling the double-sided aluminizer to 50-65 ℃, then heating to 150-. The double-sided aluminum-plated film prepared by the method has good barrier property, good adhesive force of a plating layer and high tear strength of a product.

Description

Double-sided vacuum aluminum film plating process
Technical Field
The application relates to the technical field of film coating, in particular to a double-sided vacuum aluminum film coating process.
Background
The aluminizing film is a composite flexible package material formed by plating a layer of extremely thin metal aluminum on the surface of a plastic film by adopting a special process, wherein the most common processing method is a multi-level vacuum aluminizing method, namely, the metal aluminum is melted and evaporated at high temperature in a high vacuum state, so that the vapor of the aluminum is deposited and accumulated on the surface of the plastic film, and the surface of the plastic film has metal luster. Because it has the characteristics of both plastic film and metal, it is a film material with excellent performance and strong practicability.
In the related technology, the vacuum aluminum plating process usually directly plates an aluminum layer on the surface of a substrate, during vacuum evaporation, the substrate is installed in a vacuum evaporation machine, an evaporation boat is heated to 1300 ℃, then an aluminum wire is continuously conveyed to the evaporation boat, so that the aluminum wire is continuously melted and evaporated on the evaporation boat, the film speed of the substrate is adjusted, and a bright aluminum layer, namely an aluminum plated film, is formed after the surface of the moving substrate is cooled.
In view of the above-mentioned related art, the inventors found that the aluminum plating film has a poor barrier property in packaging and use, and the aluminum plating layer is likely to fall off at a later stage.
Disclosure of Invention
In order to improve the barrier property of the aluminizer and reduce the shedding of the aluminizer, the application provides a double-sided vacuum aluminizer process.
The double-sided vacuum aluminum film plating process provided by the application adopts the following technical scheme:
a double-sided vacuum aluminum film plating process comprises the following preparation steps:
step one, melting an aluminum wire, adding trilauryl phosphite according to the proportion of 1-3wt% based on the aluminum wire, uniformly mixing, preserving heat for 20-40min, cooling to below 60 ℃, and performing vacuum sintering to obtain an aluminum material;
step two, uniformly mixing a zirconium oxychloride aqueous solution, polypropylene chloride and amantadine hydrochloride, heating to 70-85 ℃ for reaction for 50-70min to prepare a mixed glue solution, adding a tetraethylammonium chloride aqueous solution into the mixed glue solution, heating to 50-80 ℃ for reaction for 20-35min to prepare a composite glue solution, coating the composite glue solution on a base material, and then heating while performing irradiation treatment until the water is evaporated to dryness to prepare a base film;
step three, one-time vacuum evaporation: installing the base film into a vacuum evaporation machine, and carrying out single-side vacuum evaporation on the base film, wherein the thickness of a plating layer is 800-1000 angstroms, so as to obtain a single-side aluminizer;
placing the single-sided aluminizer on an aluminizing drum and rewinding for one time;
step five, secondary vacuum evaporation: carrying out vacuum evaporation on the rewound single-sided aluminizer again, wherein the thickness of the coating is 500-600 angstroms, and obtaining the double-sided aluminizer;
step six, thinning the double-sided aluminizer: uniformly cooling the double-sided aluminizer to 50-65 ℃, then heating to 150-.
By adopting the technical scheme, the aluminum wire is melted and added with the trilauryl phosphite, so that free radical polymerization is effectively prevented, other metal impurity ions contained in the aluminum wire sold in the market can be chelated, the oxidation resistance and stability of the aluminum material are improved, the phenomenon of local segregation during aluminum plating is reduced, the product is further prevented from being oxidized and discolored, the product is prevented from being blackened and faded due to oxidation, and the glossiness of the product is improved. The aluminum material is subjected to vacuum sintering, the arrangement of internal molecules is optimized, and the compactness of the formed aluminum material is improved, so that the barrier property and the tear strength of the aluminum-plated film are improved.
Mixing zirconium oxychloride aqueous solution, chlorinated polypropylene and amantadine hydrochloride for reaction, and then adding tetraethylammonium chloride aqueous solution to prepare composite glue solution, wherein the composite glue solution has good thixotropy and good compositing property with a base material; the composite glue solution can enable the surface of the base material to form a multifunctional film layer, the adhesion between the base film and the coating is effectively improved, the amantadine hydrochloride molecules simultaneously contain hydrophilic amino groups and lipophilic adamantyl groups, the surface modification can be carried out on chlorinated polypropylene, the modification effect of the composite glue solution on the surface of the base material can be promoted, the composite glue solution is further induced and modified by being coated and combined with irradiation treatment, and the tear strength of the coating is further improved.
Because the high molecular material is a poor thermal conductor, partial heat can be locked inside in the aluminizing process, and the base film is rewound once on the aluminizing drum after being subjected to vacuum evaporation once, so that the heat can be quickly dissipated, the thermal deformation can be reduced, and the quality of the aluminized film can be ensured.
And (3) immediately carrying out refining treatment after the secondary evaporation, firstly cooling to 50-65 ℃, then heating, and adopting a mode of firstly cooling and then heating, and combining irradiation treatment to facilitate the induction of intermolecular arrangement, so that the adhesiveness between the base film and the coating is stronger, and the strength of the aluminizer is better.
Preferably, in the first step, the temperature is raised to 600-650 ℃ under the vacuum sintering process condition according to 5-7 ℃/min, the temperature is kept for 1-2h, and then the temperature is cooled to below 60 ℃.
By adopting the technical scheme, the vacuum sintering process is optimized, so that arrangement of partial molecules in the aluminum material is facilitated, the compactness of the aluminum material is improved, and the barrier property of the aluminizer is further improved.
Preferably, in the second step, the mass concentration of the zirconium oxychloride aqueous solution is 5-15%, and the mass concentration of the tetraethylammonium chloride aqueous solution is 10-20%.
Preferably, in the second step, the ratio of the zirconium oxychloride aqueous solution to the polypropylene chloride aqueous solution to the amantadine hydrochloride aqueous solution to the tetraethylammonium chloride aqueous solution is 3L: (1.5-3) kg: (0.2-0.6) kg: (1-2) L.
By adopting the technical scheme, the concentrations of the zirconium oxychloride aqueous solution and the tetraethylammonium chloride aqueous solution are optimized, and the dosage ratio of the zirconium oxychloride aqueous solution, the polypropylene chloride, the amantadine hydrochloride and the tetraethylammonium chloride aqueous solution is optimized, so that the modification force of the prepared composite glue solution on the surface of the base material is further improved, and the adhesive force between the base material and the aluminized layer and the tear strength of the aluminized film are improved.
Preferably, in the second step, after the substrate is coated with the composite glue solution, the substrate is heated to 70-80 ℃, and is irradiated by gamma rays, wherein the radiation dose is 4-9 kGy/h.
By adopting the technical scheme, the heating temperature and the irradiation dose are optimized to reduce the phenomena of bubbles and shrinkage cavities generated in the process of evaporating water to dryness, so that the improvement of the composite property between the prepared composite glue solution and the base material is facilitated, and meanwhile, the surface of the base material is well modified.
Preferably, in the sixth step, the radiation dose is 6-12kGy/h by adopting gamma ray radiation.
By adopting the technical scheme, gamma rays are adopted for irradiation in the cooling and heating processes of the double-sided aluminizer, so that the arrangement among molecules is favorably induced, the viscosity between the base film and the coating is stronger, and the strength of the aluminizer is better.
Preferably, in the third step, the step of one-time vacuum evaporation specifically comprises: at 4 × E-4Evaporating and preheating to 1400-1600 ℃ in vacuum below mbar, raising the membrane speed to 220m/min, half opening the baffle, fully opening the baffle after 10s, and simultaneously lowering the membrane speed to 180m/min at 170-1600 ℃.
Through adopting above-mentioned technical scheme, optimize the technological condition of once vacuum evaporation plating, guarantee the thickness of aluminizing layer, the condition of opening and shutting of adjusting the baffle simultaneously to make the heat distribution release of preheating in-process gathering, avoid the heat scald of release in the twinkling of an eye to scald even scald the broken base film, guarantee the quality of aluminizing film.
Preferably, in the fifth step, the secondary vacuum evaporation step specifically includes: evaporating and preheating to 1400-1600 ℃ in vacuum of less than 4E-4 mbar, raising the membrane speed to 320m/min at 300-.
By adopting the technical scheme, in the secondary evaporation process, the film speed is increased so as to ensure the proper thickness of the aluminum plating layer.
Preferably, in the fourth step, the temperature of the aluminum plating drum is less than or equal to 0 ℃.
By adopting the technical scheme, the temperature of the aluminizing drum is optimized, so that the single-side aluminized film subjected to one-time vacuum evaporation is cooled quickly, and the thermal deformation is reduced.
In summary, the present application has the following beneficial effects:
1. the aluminum wire is melted and added with the trilauryl phosphite, so that free radical polymerization is effectively prevented, other metal impurity ions contained in the aluminum wire sold in the market can be chelated, the oxidation resistance and stability of the aluminum material are improved, the phenomenon of local partial aggregation during aluminum plating is reduced, the product is further prevented from being oxidized and discolored, the product is prevented from being blackened and faded due to oxidation, and the glossiness of the product is improved. The aluminum material is subjected to vacuum sintering, the arrangement of internal molecules is optimized, and the compactness of the formed aluminum material is improved, so that the barrier property and the tear strength of the aluminum-plated film are improved.
2. The surface of the base material is modified by the composite glue solution, and induced modification is carried out by combining irradiation treatment, so that a multifunctional film layer is formed on the surface of the base material, the adhesive force between the base film and the coating is effectively improved, and the tear resistance of the coating is improved.
3. The secondary evaporation is immediately refined after being finished, the film is cooled and then heated, and irradiation treatment is adopted in the process, so that intermolecular arrangement is favorably induced, the adhesiveness between the base film and the plating layer is stronger, and the strength of the aluminizer is better.
Detailed Description
The present application will be described in further detail with reference to examples.
The raw materials used in the application are common commercial raw materials, wherein the content of amantadine hydrochloride CAS number 665-66-7 is more than or equal to 98.5%, and the chlorinated polyethylene contains 40% of chlorine.
Examples
Example 1
A double-sided vacuum aluminum film plating process is prepared by the following steps:
step one, melting 1kg of aluminum wire, adding 10g of trilauryl phosphite, uniformly mixing, preserving heat for 40min, cooling to below 60 ℃, carrying out vacuum sintering, heating to 600 ℃ at a speed of 5-7 ℃/min, preserving heat for 2h, and naturally cooling to below 60 ℃ to obtain the aluminum material;
step two, uniformly mixing 3L of a zirconium oxychloride aqueous solution with the mass concentration of 15%, 1.5kg of chlorinated polypropylene and 0.2kg of amantadine hydrochloride, heating to 70 ℃ for reaction for 70min to prepare a mixed glue solution, adding 1L of a tetraethylammonium chloride aqueous solution with the mass concentration of 20% into the mixed glue solution, heating to 80 ℃ for reaction for 20min to prepare a composite glue solution, coating the composite glue solution on a base material, heating to 70 ℃, simultaneously performing irradiation treatment by adopting gamma rays with the radiation dose of 9kGy/h until the water is evaporated to dryness to prepare a base film;
step three, one-time vacuum evaporation: mounting the base film in a vacuum evaporator at 4 × E-4Evaporating and preheating to 1400 ℃ in vacuum below mbar, conveying aluminum materials into a vacuum aluminum plating machine, increasing the film speed to 220m/min, half opening a baffle, fully opening the baffle after 10s, and simultaneously reducing the film speed to 170m/min, wherein the coating thickness is 800 angstroms, so as to obtain a single-sided aluminum-plated film;
placing the single-sided aluminizer on an aluminizing drum and rewinding for one time, wherein the temperature of the aluminizing drum is 0 ℃;
step five, secondary vacuum evaporation: at 4 × E-4Evaporating and preheating to 1400 ℃ in vacuum below mbar, raising the film speed to 300m/min, half opening the baffle, fully opening the baffle after 10s, simultaneously lowering the film speed to 240m/min, and obtaining a double-sided aluminizer with the plating thickness of 500 angstroms;
step six, thinning the double-sided aluminizer: uniformly cooling the double-sided aluminizer to 65 ℃, heating to 150 ℃ at the heating rate of 3-5 ℃/min, irradiating the double-sided aluminizer by using gamma rays in the heating process, keeping the temperature for 3min, and naturally cooling to obtain a finished product of the double-sided aluminizer.
Example 2
A double-sided vacuum aluminum film plating process is prepared by the following steps:
step one, melting 1kg of aluminum wire, adding 30g of trilauryl phosphite, uniformly mixing, preserving heat for 40min, cooling to below 60 ℃, carrying out vacuum sintering, heating to 650 ℃ at the speed of 5-7 ℃/min, preserving heat for 2h, and naturally cooling to below 60 ℃ to obtain the aluminum material;
step two, uniformly mixing 3L of zirconium oxychloride aqueous solution with the mass concentration of 5%, 3kg of chlorinated polypropylene and 0.6kg of amantadine hydrochloride, heating to 85 ℃ for reaction for 50min to prepare mixed glue solution, adding 2L of tetraethylammonium chloride aqueous solution with the mass concentration of 10% into the mixed glue solution, heating to 50 ℃ for reaction for 35min to prepare composite glue solution, coating the composite glue solution on a substrate, heating to 80 ℃, simultaneously performing irradiation treatment by adopting gamma rays with the radiation dose of 4kGy/h until the moisture is evaporated to dryness, and preparing a base film;
step three, one-time vacuum evaporation: mounting the base film in a vacuum evaporator at 4 × E-4Evaporating and preheating to 1600 ℃ in vacuum below mbar, conveying aluminum to a vacuum aluminum plating machine, raising the film speed to 200m/min, half opening a baffle, fully opening the baffle after 10s, simultaneously lowering the film speed to 180m/min, and obtaining a single-side aluminum-plated film with the coating thickness of 1000 angstroms;
placing the single-sided aluminizer on an aluminizing drum and rewinding for one time, wherein the temperature of the aluminizing drum is-5 ℃;
step five, secondary vacuum evaporation: at 4 × E-4Evaporating and preheating to 1600 ℃ in vacuum below mbar, raising the film speed to 320m/min, half opening a baffle plate, fully opening the baffle plate after 10s, simultaneously lowering the film speed to 240m/min, and obtaining a double-sided aluminizer with the thickness of 600 angstroms;
step six, thinning the double-sided aluminizer: uniformly cooling the double-sided aluminizer to 50 ℃, heating to 200 ℃ at the heating rate of 3-5 ℃/min, irradiating the double-sided aluminizer by using gamma rays in the heating process, keeping the temperature for 2min, and naturally cooling to obtain a finished product of the double-sided aluminizer.
Example 3
A double-sided vacuum aluminum film plating process is prepared by the following steps:
step one, melting 1kg of aluminum wire, adding 30g of trilauryl phosphite, uniformly mixing, preserving heat for 40min, cooling to below 60 ℃, carrying out vacuum sintering, heating to 600 ℃ at a speed of 5-7 ℃/min, preserving heat for 1.5h, and naturally cooling to below 60 ℃ to obtain the aluminum material;
step two, uniformly mixing 3L of zirconium oxychloride aqueous solution with the mass concentration of 10%, 2.1kg of chlorinated polypropylene and 0.5kg of amantadine hydrochloride, heating to 80 ℃ for reaction for 60min to prepare mixed glue solution, adding 1.5L of tetraethylammonium chloride aqueous solution with the mass concentration of 16% into the mixed glue solution, heating to 70 ℃ for reaction for 30min to prepare composite glue solution, coating the composite glue solution on a base material, heating to 80 ℃, and simultaneously performing irradiation treatment by adopting gamma rays with the radiation dose of 7kGy/h until the moisture is evaporated to dryness to prepare a base film;
step three, vacuum evaporation for one time: mounting the base film in a vacuum evaporator at 4 × E-4Evaporating and preheating to 1400 ℃ in vacuum below mbar, feeding aluminum materials into a vacuum aluminum plating machine, increasing the film speed to 200m/min, half opening a baffle, fully opening the baffle after 10s, simultaneously reducing the film speed to 170m/min, and obtaining a single-side aluminum-plated film with the thickness of a plating layer of 1000 angstroms;
placing the single-sided aluminizer on an aluminizing drum and rewinding for one time, wherein the temperature of the aluminizing drum is 0 ℃;
step five, secondary vacuum evaporation: at 4 × E-4Evaporating and preheating to 1400 ℃ in vacuum below mbar, raising the film speed to 320m/min, half opening a baffle, fully opening the baffle after 10s, simultaneously reducing the film speed to 260m/min, and obtaining a double-sided aluminizer with the thickness of a plating layer of 600 angstroms;
step six, thinning the double-sided aluminizer: uniformly cooling the double-sided aluminizer to 60 ℃, heating to 160 ℃ at the heating rate of 3-5 ℃/min, irradiating the double-sided aluminizer by using gamma rays in the heating process, keeping the temperature for 3min, and naturally cooling to obtain a finished product of the double-sided aluminizer.
Example 4
The difference from the embodiment 3 is that the first step is different from the first step, and the first step specifically comprises the following steps: melting 1kg of aluminum wire, adding 30g of trilauryl phosphite, uniformly mixing, preserving heat for 40min, cooling to below 60 ℃, performing vacuum sintering, heating to 400 ℃ at the speed of 5-7 ℃/min, preserving heat for 1.5h, and naturally cooling to below 60 ℃ to obtain the aluminum material; the rest is the same as in example 3.
Example 5
The difference from the embodiment 3 is that the second step is different, and the second step specifically comprises the following steps: uniformly mixing 3L of zirconium oxychloride aqueous solution with the mass concentration of 30%, 2.1kg of polypropylene chloride and 0.5kg of amantadine hydrochloride, heating to 80 ℃ for reaction for 60min to prepare mixed glue solution, adding 1.5L of tetraethylammonium chloride aqueous solution with the mass concentration of 5% into the mixed glue solution, heating to 70 ℃ for reaction for 30min to prepare composite glue solution, coating the composite glue solution on a substrate, heating to 80 ℃, simultaneously performing irradiation treatment by adopting gamma rays with the radiation dose of 7kGy/h until the moisture is evaporated to dryness to prepare a base film; the rest is the same as in example 3.
Example 6
The difference from the embodiment 3 is that the second step is different, and the second step specifically comprises the following steps: uniformly mixing 5L of zirconium oxychloride aqueous solution with the mass concentration of 10%, 1kg of polypropylene chloride and 1kg of amantadine hydrochloride, heating to 80 ℃ for reaction for 60min to prepare mixed glue solution, adding 0.5L of tetraethyl ammonium chloride aqueous solution with the mass concentration of 16% into the mixed glue solution, heating to 70 ℃ for reaction for 30min to prepare composite glue solution, coating the composite glue solution on a base material, heating to 80 ℃, simultaneously performing irradiation treatment by adopting gamma rays with the radiation dose of 7kGy/h until the water is evaporated to dryness to prepare a base film; the rest is the same as in example 3.
Example 7
The difference from the embodiment 3 is that the second step is different, and the second step specifically comprises the following steps: uniformly mixing 3L of zirconium oxychloride aqueous solution with the mass concentration of 10%, 2.1kg of polypropylene chloride and 0.5kg of amantadine hydrochloride, heating to 80 ℃ for reaction for 60min to prepare mixed glue solution, adding 1.5L of tetraethylammonium chloride aqueous solution with the mass concentration of 16% into the mixed glue solution, heating to 70 ℃ for reaction for 30min to prepare composite glue solution, coating the composite glue solution on a substrate, heating to 100 ℃, and simultaneously performing irradiation treatment by adopting X rays with the radiation dose of 11kGy/h until the moisture is evaporated to dryness to prepare a base film; the rest is the same as in example 3.
Example 8
The difference from the embodiment 3 is that the third step is different from the fifth step, and the third step specifically comprises the following steps: primary vacuum evaporation: mounting the base film in a vacuum evaporator at 4 × E-4Evaporating and preheating to 1200 ℃ in vacuum below mbar, feeding aluminum material into a vacuum aluminum plating machine, raising the film speed to 200m/min, fully opening a baffle plate, and obtaining a single-side aluminum plating film, wherein the thickness of a plating layer is 1000 angstroms;
the fifth step is specifically as follows: secondary vacuum evaporation: at 4 × E-4Evaporating and preheating to 1200 ℃ in vacuum below mbar, raising the film speed to 320m/min, fully opening a baffle plate, and obtaining a double-sided aluminizer with the thickness of a plating layer of 600 angstroms; the rest was the same as in example 3.
Example 9
The difference from the embodiment 3 is that the sixth step is different from the first step, and specifically: thinning the double-sided aluminizer: uniformly cooling the double-sided aluminizer to 60 ℃, heating to 160 ℃ at the heating rate of 3-5 ℃/min, irradiating the double-sided aluminizer by using a 400W ultraviolet lamp in the heating process, preserving heat for 3min, and naturally cooling to obtain a double-sided aluminizer finished product; the rest is the same as in example 3.
Comparative example
Comparative example 1
A double-sided vacuum aluminum film plating process is prepared by the following steps:
step one, vacuum evaporation plating: mounting the base film in a vacuum evaporator at 4 × E-4Evaporating and preheating to 1400 deg.C in vacuum below mbar, feeding aluminum material into vacuum aluminum plating machine, increasing film speed to 200m/min, half opening baffle, fully opening baffle after 10s,simultaneously, the film speed is reduced to 170m/min, the thickness of the plating layer is 1000 angstroms, and a single-side aluminizer is obtained;
placing the single-sided aluminizer on an aluminizing drum and rewinding for one time, wherein the temperature of the aluminizing drum is 0 ℃;
step three, secondary vacuum evaporation: at 4 × E-4Evaporating and preheating to 1400 ℃ in vacuum below mbar, raising the film speed to 320m/min, half opening the baffle, fully opening the baffle after 10s, simultaneously lowering the film speed to 260m/min, and obtaining the double-sided aluminizer with the plating thickness of 600 angstroms.
Comparative example 2
The difference from example 1 is that step one is omitted, and the aluminum wire is used without being treated, and the rest is the same as example 1.
Comparative example 3
The difference from the embodiment 1 is that the second step is omitted; the rest is the same as in example 1.
Comparative example 4
The difference from example 1 is that step two is different, and no amantadine hydrochloride is added in step two, and the rest is the same as example 1.
Comparative example 5
The difference from the embodiment 1 is that the sixth step is omitted, the double-sided aluminizer is not subjected to thinning treatment, and the rest is the same as the embodiment 1.
Comparative example 6
The difference from the embodiment 1 is that the step six is different, and the step six specifically comprises the following steps: thinning the double-sided aluminizer: uniformly cooling the double-sided aluminizer to room temperature, heating to 160 ℃ at a heating rate of 3-5 ℃/min, and naturally cooling to obtain a double-sided aluminizer finished product; the rest is the same as in example 1.
Comparative example 7
The difference from the example 1 is that in the fourth step, the temperature of the aluminum plating drum is 20 ℃; the rest is the same as in example 1.
Performance test
The examples 1 to 9 and comparative examples 1 to 7 were tested for water vapor permeability, oxygen permeability, tensile strength, and adhesion of the aluminum plating layer (expressed as an area where the aluminum plating layer was peeled) in accordance with BB/T0030-.
TABLE 1 test results
Figure BDA0003367608560000121
Figure BDA0003367608560000131
By combining the examples 1 to 3 and the table 1, it can be seen that the aluminum-plated film with excellent performance can be prepared by properly adjusting the process parameters of the steps, and the aluminum-plated film has excellent barrier property, tear strength, good adhesion of the aluminum layer and no falling-off phenomenon. It can be seen from examples 3 and 4 that the sintering temperature was adjusted to 400 ℃, which did not provide a good sintering effect, and which had a certain effect on the compactness of the formed aluminum material and the barrier property of the aluminum plated film, and the aluminum plated layer was slightly peeled off. It can be seen from the examples 3 and 5-6 and table 1 that the concentrations of the zirconium oxychloride aqueous solution and the tetraethylammonium chloride aqueous solution in example 5 are unbalanced, and the ratio of the raw material components in example 6 is unbalanced, which results in the decrease of the modification effect of the composite glue solution on the base material, the decrease of the compound property, the decrease of the adhesion of the coating, and the falling of the coating to a certain extent, and thus it can be seen that the raw material components of the composite glue solution can play a better role only at a certain ratio.
As can be seen from examples 3 and 7 in combination with table 1, in example 7, the substrate was taken out and heated to 100 ℃, and X-rays were used for irradiation, so that moisture was evaporated too quickly, fine micropores were generated on the surface of the aluminum film, and the X-rays could not play a good inducing role, so that the barrier property of the aluminum plated film was poor, the oxygen permeation amount and the water vapor permeation amount were both increased, the peeling area of the aluminum plated layer was also increased, and the adhesion of the aluminum plated layer was decreased.
As can be seen from the examples 3 and 8 and the table 1, the process parameters of the first vacuum evaporation and the second vacuum evaporation are adjusted, the evaporation preheating temperature is adjusted to 1200 ℃, the baffle is directly opened completely, and the film speed is not adjusted, so that the whole aluminum-plated layer has certain thermal deformation, and the aluminum-plated layer also has a certain segregation phenomenon, so that the aluminum-plated film is influenced to a certain extent regardless of the barrier property, the tensile strength and the adhesion of the plating layer.
As can be seen from the examples 3 and 9 in combination with table 1, in the refinement treatment of the double-sided aluminum-plated film, the ultraviolet irradiation treatment is performed on the double-sided aluminum-plated film in example 9, which does not have a good refinement effect on the aluminum-plated film, so that the oxygen transmission amount and the water vapor transmission amount of the aluminum-plated film are both increased, the aluminum layer falling area is increased, and the adhesion of the aluminum-plated film is reduced to a certain extent.
As can be seen from the combination of example 1 and comparative example 1 and table 1, the double-sided aluminum plating film manufactured by the most common double-sided aluminum plating method has a low oxygen transmission amount and a low water vapor transmission amount, has excellent barrier property, and has excellent tear strength, good adhesion of the aluminum plating layer, and no peeling, compared to the double-sided aluminum plating film manufactured by the present application.
It can be seen from the combination of example 1 and comparative example 2 and table 1 that step one is omitted, the aluminum wire is directly used without any treatment, and the aluminum wire cannot be compounded and cooperated with the multifunctional composite film formed on the surface of the base material by the composite glue solution in step two, and local segregation is easy to occur during evaporation, the disordered arrangement among molecules is large, the compactness of the aluminum plated layer is reduced, the water vapor permeability and the oxygen permeability are obviously increased, and the adhesion between the aluminum plated layer and the base film is affected, so that the shedding area of the aluminum plated layer is increased.
By combining the example 1 and the comparative examples 3 to 4 and combining the table 1, it can be seen that the treatment of the second step is omitted in the comparative example 3, the surface of the base material is modified and decorated by the composite glue solution, the barrier property of the aluminizer is poor, and the adhesive force between the base film and the plating layer and the tear strength of the plating layer cannot be effectively improved; comparative example 4 amantadine hydrochloride was not added in step two, the acting force of the synergistic treatment among the raw material components was weakened, the modification and modification effects of the composite glue solution on the surface of the base film were weakened, and the performances of the aluminized films worthy of comparative examples 3 and 4 were all significantly reduced.
It can be seen by combining example 1 and comparative examples 5 to 6 with table 1 that comparative example 5 is directly not subjected to the thinning treatment, comparative example 6 is cooled to room temperature and then heated in the thinning process, but is not subjected to the irradiation treatment in the heating process, and the performance of the aluminum plated films prepared in comparative example 5 and comparative example 6 is not good enough, so that the quality of the aluminum plated film can be synergistically improved by firstly cooling to a specific temperature in the thinning process and then heating and combining the irradiation treatment. By combining the example 1 and the comparative example 7 and combining the table 1, the temperature of the aluminizing drum of the comparative example 7 is adjusted to 20 ℃, the temperature cannot be rapidly reduced, and part of heat is locked inside, so that the product has some thermal deformation, and the tensile strength and the coating adhesion of the aluminizing film are greatly influenced.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.

Claims (9)

1. A double-sided vacuum aluminum film plating process is characterized by comprising the following preparation steps:
step one, melting an aluminum wire, adding trilauryl phosphite according to the proportion of 1-3wt% based on the aluminum wire, uniformly mixing, keeping the temperature for 20-40min, cooling to below 60 ℃, and performing vacuum sintering to obtain an aluminum material;
step two, uniformly mixing a zirconium oxychloride aqueous solution, polypropylene chloride and amantadine hydrochloride, heating to 70-85 ℃ for reaction for 50-70min to prepare a mixed glue solution, adding a tetraethylammonium chloride aqueous solution into the mixed glue solution, heating to 50-80 ℃ for reaction for 20-35min to prepare a composite glue solution, coating the composite glue solution on a substrate, and then heating while performing irradiation treatment until the water is evaporated to dryness to prepare a base membrane;
step three, vacuum evaporation for one time: installing the base film into a vacuum evaporation machine, and carrying out single-side vacuum evaporation on the base film, wherein the thickness of a plating layer is 800-1000 angstroms, so as to obtain a single-side aluminizer;
placing the single-sided aluminizer on an aluminizing drum and rewinding for one time;
step five, secondary vacuum evaporation: carrying out vacuum evaporation on the rewound single-sided aluminizer again, wherein the thickness of the coating is 500-600 angstroms, and obtaining the double-sided aluminizer;
step six, thinning the double-sided aluminizer: uniformly cooling the double-sided aluminizer to 50-65 ℃, then heating to 150-200 ℃, preserving heat for 2-3min, adopting irradiation treatment in the heating process, and naturally cooling to obtain a double-sided aluminizer finished product.
2. The double-sided vacuum aluminizing process according to claim 1, characterized in that: in the first step, the temperature is raised to 600-650 ℃ according to the vacuum sintering process condition at the speed of 5-7 ℃/min, the temperature is kept for 1-2h, and then the temperature is cooled to below 60 ℃.
3. The double-sided vacuum aluminizing process according to claim 1, characterized in that: in the second step, the mass concentration of the zirconium oxychloride aqueous solution is 5-15%, and the mass concentration of the tetraethylammonium chloride aqueous solution is 10-20%.
4. The double-sided vacuum aluminizing process according to claim 1, characterized in that: in the second step, the dosage ratio of the zirconium oxychloride aqueous solution, the chlorinated polypropylene, the amantadine hydrochloride and the tetraethylammonium chloride aqueous solution is 3L: (1.5-3) kg: (0.2-0.6) kg: (1-2) L.
5. The double-sided vacuum aluminizing process according to claim 3 or 4, characterized in that: in the second step, after the substrate is coated with the composite glue solution, the substrate is heated to 70-80 ℃, and is irradiated by gamma rays, wherein the radiation dose is 4-9 kGy/h.
6. The double-sided vacuum aluminizing process according to claim 1, characterized in that: and in the sixth step, gamma rays are adopted for irradiation, and the radiation dose is 6-12 kGy/h.
7. The double-sided vacuum aluminizing process according to claim 1, characterized in that: in the third step, the step of one-time vacuum evaporation specifically comprises the following steps: at 4 × E-4Evaporating and preheating to 1400-1600 ℃ in vacuum below mbar, raising the membrane speed to 220m/min, half opening the baffle, fully opening the baffle after 10s, and simultaneously lowering the membrane speed to 180m/min at 170-1600 ℃.
8. The double-sided vacuum aluminizing process according to claim 7, characterized in that: in the fifth step, the secondary vacuum evaporation comprises the following specific steps: at 4 × E-4Evaporating and preheating to 1400-1600 ℃ in vacuum below mbar, raising the membrane speed to 320m/min at 300-1600 ℃, half opening the baffle, fully opening the baffle after 10s, and simultaneously lowering the membrane speed to 260m/min at 240-260 ℃.
9. The double-sided vacuum aluminizing process according to claim 7, characterized in that: in the fourth step, the temperature of the aluminum plating drum is less than or equal to 0 ℃.
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