CN110983259A - High-composite-strength back-side aluminum-plated VMPET film and preparation method thereof - Google Patents

High-composite-strength back-side aluminum-plated VMPET film and preparation method thereof Download PDF

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CN110983259A
CN110983259A CN201911293306.XA CN201911293306A CN110983259A CN 110983259 A CN110983259 A CN 110983259A CN 201911293306 A CN201911293306 A CN 201911293306A CN 110983259 A CN110983259 A CN 110983259A
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film
evaporation
aluminum
vmpet
composite
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曹赤鹏
魏威
孙丽霞
张建平
张伟政
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Jiaxing Pengxiang Packaging Material Co ltd
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Jiaxing Pengxiang Packaging Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02Pretreatment of the material to be coated
    • C23C14/021Cleaning or etching treatments
    • C23C14/022Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/20Metallic material, boron or silicon on organic substrates
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54Controlling or regulating the coating process
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • C23C14/562Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks for coating elongated substrates

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
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  • Metallurgy (AREA)
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Abstract

The invention discloses a preparation method of a high-composite-strength back-side aluminized VMPET film, which is characterized by comprising the following steps of: 1) unreeling the substrate; 2) turning on the capture pump; 3) vacuumizing; 4) heating the evaporation boat; 5) feeding an aluminum wire; 6) carrying out plasma treatment; 7) evaporation; 8) cooling; 9) measuring the thickness; 10) and (6) rolling. According to the high-composite-strength back side aluminized VMPET film, the technological condition parameters of all the steps are strictly controlled, the corona surface (the surface tension reaches 58-60 dyn/cm) of the PET base film is reserved for the subsequent procedure of compounding with PE, aluminizing is carried out on the non-corona surface of the PET base film, and a plasma treatment technology is applied in the aluminizing process, so that the back side aluminized VMPET film is obtained.

Description

High-composite-strength back-side aluminum-plated VMPET film and preparation method thereof
Technical Field
The invention relates to the field of vacuum aluminized film products, in particular to a high-composite-strength back aluminized VMPET film and a preparation method thereof.
Background
The VMPET film has good dimensional stability and heat resistance, excellent printing adaptability, good water and gas resistance, and can meet the requirement of the commodity on barrier property. However, the common VMPET has no heat sealing performance, and in order to solve the heat sealing problem, the VMPET is usually compounded with a heat sealing material such as PE or CPP, and then can be used for commodity packaging.
The most commonly used composite film structure in the market at present is BOPP/VMPET/PE, but the low composite strength of the VMPET/PE composite layer in the structure is a common problem, mainly because the non-corona surface of the VMPET is compounded with the PE, although the PET macromolecular chain contains polar groups, the PET macromolecular chain has certain polarity, the surface tension of the PET macromolecular chain can reach 40-44 dyn/cm generally, the common glue for compounding is polyurethane, the surface tension of the common glue is 40-60 dyn/cm generally, because of the difference of the surface tension of the common PET macromolecular chain and the non-aluminum-plated surface tension of the VMPET, the composite strength between the VMPET/PE is about 2.0N/15mm after the common PET/PE composite film is compounded, and the strength requirement of the medicine package in the market is more than 3.0N/15 mm.
At present, the surface tension of a VMPET non-aluminum-plated surface is increased by corona treatment to reach 50-54 dyn/cm, but the treatment effect is influenced by time and environment temperature and humidity, and the surface tension is reduced along with the increase of the standing time and the temperature and humidity. Therefore, the initial composite strength after the composition with PE can reach 3.0N/15mm or more, but the composite strength is reduced with the passage of time.
According to the invention, the corona surface (surface tension of 58-60 dyn/cm) of the PET base film is reserved for the subsequent process of compounding with PE, aluminum plating is carried out on the non-corona surface of the PET base film, and a plasma treatment technology is applied in the aluminum plating process to obtain the back side aluminum-plated VMPET film.
Disclosure of Invention
The invention aims to provide a reverse side aluminized VMPET film with high composite strength and a preparation method thereof. According to the high-composite-strength back side aluminized VMPET film, the technological condition parameters of all the steps are strictly controlled, the corona surface (the surface tension reaches 58-60 dyn/cm) of the PET base film is reserved for the subsequent procedure of compounding with PE, aluminizing is carried out on the non-corona surface of the PET base film, and a plasma treatment technology is applied in the aluminizing process, so that the back side aluminized VMPET film is obtained.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of a reverse side aluminized VMPET film with high composite strength is characterized by comprising the following steps:
1) unreeling the substrate;
2) turning on the capture pump;
after the substrate film is unreeled, closing a bin body of a vacuum bin of the aluminum plating machine, opening a capture pump before vacuumizing, and condensing water in the vacuum bin of the aluminum plating machine into ice through the capture pump;
3) vacuumizing;
vacuumizing a vacuum bin of the aluminum plating machine and maintaining the vacuum degree to be 10-4 mbar;
4) heating the evaporation boat;
the time for starting heating the evaporation boat to normal evaporation is controlled to be 12-16 minutes in principle. The evaporation boat is heated in 4 stages, each stage takes 3-4 minutes, the power is 0-40%, 40-50%, 50-70% and 70-80% respectively, meanwhile, the voltage of the evaporation boat is increased by no more than 1V compared with the ordinary normal heating during the first heating, and the voltage is reduced after the evaporation boat is normally evaporated, so that the aluminum liquid spreading area of the evaporation boat can be increased, and the evaporation efficiency is improved.
5) Feeding an aluminum wire;
when the aluminum wires in the boat grooves of the evaporation boat are melted, the temperature of each boat is adjusted until the temperature of all the boats is adjusted to be within +/-0.1 ℃ (basically the same);
heating the evaporation boat and feeding the wire can be carried out cooperatively.
6) Carrying out plasma treatment;
the surface of the base material film is treated at the running speed of 12-14 m/s by mixing the oxygen flow of 200-400 sccm and the argon flow of 800-1200 sccm, controlling the current intensity of 15-20A, the purity of the plasma substance of more than 99.9 percent and the flow of the plasma substance of 500-1000 sccm, and increasing the adhesion fastness of the aluminum layer on the surface of the film.
The plasma treatment can remove pollutants and residual gas on the surface of the aluminum-plated substrate, effectively avoid the generation of micro pinholes on the aluminum layer due to gas release in the aluminum-plating process, and enhance the compactness of the aluminum layer. On the other hand, a certain amount of polar groups such as-CO, -OH, -COOH, -NH and the like can be formed on the non-corona surface of the PET film, so that the surface activity of the base material can be greatly improved. The treated surface of the base material is easy to form firm and compact binding force with Van der Waals force, hydrogen bonds or chemical bonds, so that the adhesive force of the aluminum layer is obviously improved.
7) Evaporation;
the evaporation boat is fixed on the holder for heating during evaporation; during normal production, the temperature of the evaporation boat is 1300-1400 ℃, and step 5) is carried out simultaneously to continuously send the high-purity aluminum wire to the evaporation boat by the conveying motor and gasify the aluminum wire;
in the evaporation process, attention must be paid to control the temperature of the evaporation boat, and the service life of the evaporation boat is seriously influenced by overhigh or overlow temperature. The method comprises the steps of observing the spreading area of aluminum liquid in a boat tank and whether the aluminum liquid is boiled or not by naked eyes in the evaporation process, finding out the uniformity of aluminum plating through an observation window, judging whether the temperature of the boat is too high or too dripping or not, if the spreading area of the aluminum liquid is reduced, the phenomenon of aluminum splashing exists, the uniformity of the thickness of an aluminum layer is not enough, considering that the temperature of the evaporation boat is too high, and reducing the temperature of the evaporation boat.
8) Cooling;
and cooling while evaporating, wherein the cooling temperature is 0-3 ℃.
9) Measuring the thickness;
measuring a square resistance value through a continuous non-contact measurement thin film metal coating thickness system, calculating the higher or lower square resistance value according to the set square resistance value, and adjusting the thickness of the aluminum layer according to the higher or lower square resistance value in time;
10) rolling;
the rolling tension is adjusted to ensure that the film is spread flatly without edge slipping and rib breaking.
According to the high-composite-strength back side aluminized VMPET film, the technological condition parameters of all the steps are strictly controlled, the corona surface (the surface tension reaches 58-60 dyn/cm) of the PET base film is reserved for the subsequent procedure of compounding with PE, aluminizing is carried out on the non-corona surface of the PET base film, and a plasma treatment technology is applied in the aluminizing process, so that the back side aluminized VMPET film is obtained.
The high-composite-strength back-side aluminized VMPET film is obtained by heating and melting aluminum metal to be evaporated on a non-corona surface of a PET base film under the vacuum degree of more than 10-4mbar, condensing aluminum atoms on the non-corona surface of the PET to form an extremely thin aluminum layer and rolling the extremely thin aluminum layer.
According to the high-composite-strength back-side aluminized VMPET film, aluminizing is performed on the non-corona surface of the PET base film, the corona surface (the surface tension reaches 58-60 dyn/cm) of the base film is reserved for the subsequent composite process, the polyurethane adhesive can be well dispersed on the non-aluminized surface of the VMPET, and the composite strength is improved.
In the vacuum aluminum plating process, in order to improve the wetting tension of the non-corona surface of the PET and facilitate the aluminum plating, a plasma treatment process is applied, so that the aluminum layer can obtain good adhesive force even if the non-corona surface is plated with aluminum.
In the invention, different aluminum layer adhesive forces can be obtained by adjusting different gas flow rates and current values of plasma treatment, so that the film is more widely applied.
Preferably, in the step 1), the unreeling of the substrate is to continuously unreel the substrate film through each guide roller according to a path required for vacuum aluminizing.
Preferably, in step 1), the substrate film is a polyester film.
Preferably, in step 1), the substrate film is a PET film.
Preferably, in step 2), the temperature of the capture pump is controlled to-150. + -. 5 ℃. Therefore, the vacuum pumping is facilitated, the workload of the collecting pump can be reduced, and the energy-saving and environment-friendly effects are achieved.
Preferably, in the step 3), the vacuum pumping process is divided into three stages, firstly, the mechanical pump is used for primary pumping, then the roots pump works, when the vacuum degree in the vacuum chamber reaches 10-2mbar, the diffusion pump is opened, and the high vacuum degree in the vacuum chamber, namely 10-4mbar, is further improved and maintained by the diffusion pump so as to meet the requirement of evaporation production.
Preferably, in step 4), the evaporation boat is heated in 4 stages, each stage takes 3.5 minutes, the power is 20%, 45%, 60% and 75%, meanwhile, the voltage of the evaporation boat is increased by no more than 1V compared with the ordinary normal heating during the first heating, and the voltage is reduced after the evaporation boat is normally evaporated, so that the aluminum liquid spreading area of the evaporation boat can be increased, and the evaporation efficiency is improved.
Preferably, in the step 6), the surface of the substrate film is treated at the running speed of 13m/s by mixing the oxygen flow rate of 300sccm and the argon flow rate of 1000sccm, controlling the current intensity of 18A, the purity of the plasma substance to be more than 99.9 percent and the flow rate of the plasma substance to be 750sccm, so as to increase the adhesion fastness of the aluminum layer on the surface of the film.
The invention also provides a high-composite-strength reverse side aluminum-plated VMPET film, which is prepared by adopting the preparation method of the high-composite-strength reverse side aluminum-plated VMPET film.
Compared with the prior art, the invention has the following advantages and beneficial effects:
according to the high-composite-strength back side aluminized VMPET film, the technological condition parameters of all the steps are strictly controlled, the corona surface (the surface tension reaches 58-60 dyn/cm) of the PET base film is reserved for the subsequent procedure of compounding with PE, aluminizing is carried out on the non-corona surface of the PET base film, and a plasma treatment technology is applied in the aluminizing process, so that the back side aluminized VMPET film is obtained.
The high-composite-strength back-side aluminized VMPET film is obtained by heating and melting aluminum metal to be evaporated on a non-corona surface of a PET base film under the vacuum degree of more than 10-4mbar, condensing aluminum atoms on the non-corona surface of the PET to form an extremely thin aluminum layer and rolling the extremely thin aluminum layer.
According to the high-composite-strength back-side aluminized VMPET film, aluminizing is performed on the non-corona surface of the PET base film, the corona surface (the surface tension reaches 58-60 dyn/cm) of the base film is reserved for the subsequent composite process, the polyurethane adhesive can be well dispersed on the non-aluminized surface of the VMPET, and the composite strength is improved.
In the vacuum aluminum plating process, in order to improve the wetting tension of the non-corona surface of the PET and facilitate the aluminum plating, a plasma treatment process is applied, so that the aluminum layer can obtain good adhesive force even if the non-corona surface is plated with aluminum.
In the invention, different aluminum layer adhesive forces can be obtained by adjusting different gas flow rates and current values of plasma treatment, so that the film is more widely applied.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, the following description of the preferred embodiments of the present invention is provided in connection with specific examples, which should not be construed as limiting the present patent.
The test methods or test methods described in the following examples are conventional methods unless otherwise specified; the reagents and materials, unless otherwise indicated, are conventionally obtained commercially or prepared by conventional methods.
Example 1:
a preparation method of a reverse side aluminized VMPET film with high composite strength is characterized by comprising the following steps:
1) unreeling the substrate;
2) turning on the capture pump;
after the substrate film is unreeled, closing a bin body of a vacuum bin of the aluminum plating machine, opening a capture pump before vacuumizing, and condensing water in the vacuum bin of the aluminum plating machine into ice through the capture pump;
3) vacuumizing;
vacuumizing a vacuum bin of the aluminum plating machine and maintaining the vacuum degree to be 10-4 mbar;
4) heating the evaporation boat;
the time for starting heating the evaporation boat to normal evaporation is controlled to be 12-16 minutes in principle. The evaporation boat is heated in 4 stages, each stage takes 3-4 minutes, the power is 0-40%, 40-50%, 50-70% and 70-80%, meanwhile, the evaporation boat is heated for the first time, the voltage is increased by no more than 1V compared with the ordinary normal heating, and the voltage is reduced after the evaporation boat is normally evaporated;
5) feeding an aluminum wire;
when the aluminum wires in the boat grooves of the evaporation boat are melted, the temperature of each boat is adjusted until the temperature of all the boats is adjusted to be within +/-0.1 ℃ (basically the same);
6) carrying out plasma treatment;
mixing oxygen flow of 200-400 sccm and argon flow of 800-1200 sccm, controlling current intensity of 15-20A, purity of plasma substance of more than 99.9% and flow of plasma substance of 500-1000 sccm, and treating the surface of the substrate film at a running speed of 12-14 m/s;
7) evaporation;
the evaporation boat is fixed on the holder for heating during evaporation; during normal production, the temperature of the evaporation boat is 1300-1400 ℃, and step 5) is carried out simultaneously to continuously send the high-purity aluminum wire to the evaporation boat by the conveying motor and gasify the aluminum wire;
8) cooling;
cooling while evaporating, wherein the cooling temperature is 0-3 ℃;
9) measuring the thickness;
measuring a square resistance value through a continuous non-contact measurement thin film metal coating thickness system, calculating the higher or lower square resistance value according to the set square resistance value, and adjusting the thickness of the aluminum layer according to the higher or lower square resistance value in time;
10) rolling;
the rolling tension is adjusted to ensure that the film is spread flatly without edge slipping and rib breaking.
Preferably, in the step 1), the unreeling of the substrate is to continuously unreel the substrate film through each guide roller according to a path required for vacuum aluminizing.
Preferably, in step 1), the substrate film is a polyester film.
Preferably, in step 1), the substrate film is a PET film.
Preferably, in step 2), the temperature of the capture pump is controlled to-150. + -. 5 ℃. Therefore, the vacuum pumping is facilitated, the workload of the collecting pump can be reduced, and the energy-saving and environment-friendly effects are achieved.
Preferably, in the step 3), the vacuum pumping process is divided into three stages, firstly, the mechanical pump is used for primary pumping, then the roots pump works, when the vacuum degree in the vacuum chamber reaches 10-2mbar, the diffusion pump is opened, and the high vacuum degree in the vacuum chamber, namely 10-4mbar, is further improved and maintained by the diffusion pump so as to meet the requirement of evaporation production.
Preferably, in step 4), the evaporation boat is heated in 4 stages, each stage takes 3.5 minutes, the power is 20%, 45%, 60% and 75%, meanwhile, the voltage of the evaporation boat is increased by no more than 1V compared with the ordinary normal heating during the first heating, and the voltage is reduced after the evaporation boat is normally evaporated, so that the aluminum liquid spreading area of the evaporation boat can be increased, and the evaporation efficiency is improved.
Preferably, in the step 6), the surface of the substrate film is treated at the running speed of 13m/s by mixing the oxygen flow rate of 300sccm and the argon flow rate of 1000sccm, controlling the current intensity of 18A, the purity of the plasma substance to be more than 99.9 percent and the flow rate of the plasma substance to be 750sccm, so as to increase the adhesion fastness of the aluminum layer on the surface of the film.
The invention also provides a high-composite-strength reverse side aluminum-plated VMPET film, which is prepared by adopting the preparation method of the high-composite-strength reverse side aluminum-plated VMPET film.
Example 2:
a preparation method of a reverse side aluminized VMPET film with high composite strength is characterized by comprising the following steps:
1) unreeling the substrate;
2) turning on the capture pump;
after the substrate film is unreeled, closing a bin body of a vacuum bin of the aluminum plating machine, opening a capture pump before vacuumizing, and condensing water in the vacuum bin of the aluminum plating machine into ice through the capture pump;
3) vacuumizing;
vacuumizing a vacuum bin of the aluminum plating machine and maintaining the vacuum degree to be 10-4 mbar;
4) heating the evaporation boat;
the time period from the start of heating the evaporation boat to normal evaporation was controlled to 12 minutes in principle. The evaporation boat is heated in 4 stages, each stage takes 3 minutes, the power is 40%, 50%, 70% and 80%, meanwhile, the evaporation boat is heated for the first time, the voltage is increased by no more than 1V compared with the ordinary normal heating, and the voltage is reduced after the evaporation is performed normally;
5) feeding an aluminum wire;
when the aluminum wires in the boat grooves of the evaporation boat are melted, the temperature of each boat is adjusted until the temperature of all the boats is adjusted to be within +/-0.1 ℃ (basically the same);
6) carrying out plasma treatment;
the surface of the substrate film is treated at the running speed of 12m/s by mixing the oxygen flow of 200sccm and the argon flow of 800sccm, controlling the current intensity to be 15A, the purity of the plasma substance to be more than 99.9 percent and the flow of the plasma substance to be 500 sccm;
7) evaporation;
the evaporation boat is fixed on the holder for heating during evaporation; during normal production, the temperature of the evaporation boat is 1300 ℃, and simultaneously, the step 5) is carried out to continuously send the high-purity aluminum wire to the evaporation boat by the conveying motor and gasify the high-purity aluminum wire;
8) cooling;
cooling while evaporating, wherein the cooling temperature is 0 ℃;
9) measuring the thickness;
measuring a square resistance value through a continuous non-contact measurement thin film metal coating thickness system, calculating the higher or lower square resistance value according to the set square resistance value, and adjusting the thickness of the aluminum layer according to the higher or lower square resistance value in time;
10) rolling;
the rolling tension is adjusted to ensure that the film is spread flatly without edge slipping and rib breaking.
In this embodiment, in step 1), the unwinding of the substrate is to continuously unwind the substrate film through each guide roller according to a path required for vacuum aluminum plating.
In this embodiment, in step 1), the substrate film is a polyester film.
In this embodiment, in step 1), the substrate film is a PET film.
In this example, the temperature of the trap pump was controlled at-155 ℃ in step 2). Therefore, the vacuum pumping is facilitated, the workload of the collecting pump can be reduced, and the energy-saving and environment-friendly effects are achieved.
In this embodiment, in step 3), the vacuum pumping process is divided into three stages, first, a mechanical pump performs primary pumping, then a roots pump works, when the vacuum degree in the vacuum chamber reaches 10-2mbar, a diffusion pump is opened, and the high vacuum degree in the vacuum chamber, namely 10-4mbar, is further improved and maintained by the diffusion pump, so as to meet the requirement of evaporation production.
In the embodiment, the reverse side aluminum-plated VMPET film with high composite strength is further provided, and is prepared by the preparation method of the reverse side aluminum-plated VMPET film with high composite strength.
Example 3:
a preparation method of a reverse side aluminized VMPET film with high composite strength is characterized by comprising the following steps:
1) unreeling the substrate;
2) turning on the capture pump;
after the substrate film is unreeled, closing a bin body of a vacuum bin of the aluminum plating machine, opening a capture pump before vacuumizing, and condensing water in the vacuum bin of the aluminum plating machine into ice through the capture pump;
3) vacuumizing;
vacuumizing a vacuum bin of the aluminum plating machine and maintaining the vacuum degree to be 10-4 mbar;
4) heating the evaporation boat;
the time period from the start of heating the evaporation boat to normal evaporation was controlled to 16 minutes in principle. The evaporation boat is heated in 4 stages, each stage takes 4 minutes, the power is 15%, 40%, 50% and 70%, meanwhile, the evaporation boat is heated for the first time, the voltage is increased by no more than 1V compared with the ordinary normal heating, and the voltage is reduced after the evaporation is performed normally;
5) feeding an aluminum wire;
when the aluminum wires in the boat grooves of the evaporation boat are melted, the temperature of each boat is adjusted until the temperature of all the boats is adjusted to be within +/-0.1 ℃ (basically the same);
6) carrying out plasma treatment;
the surface of the substrate film is treated at the running speed of 14m/s by mixing the oxygen flow of 400sccm and the argon flow of 1200sccm, controlling the current intensity to be 20A, the purity of the plasma substance to be more than 99.9 percent and the flow of the plasma substance to be 1000 sccm;
7) evaporation;
the evaporation boat is fixed on the holder for heating during evaporation; during normal production, the temperature of the evaporation boat is 1400 ℃, and step 5) is carried out simultaneously to continuously send the high-purity aluminum wire to the evaporation boat by the conveying motor and gasify the aluminum wire;
8) cooling;
cooling while evaporating, wherein the cooling temperature is 3 ℃;
9) measuring the thickness;
measuring a square resistance value through a continuous non-contact measurement thin film metal coating thickness system, calculating the higher or lower square resistance value according to the set square resistance value, and adjusting the thickness of the aluminum layer according to the higher or lower square resistance value in time;
10) rolling;
the rolling tension is adjusted to ensure that the film is spread flatly without edge slipping and rib breaking.
In this embodiment, in step 1), the unwinding of the substrate is to continuously unwind the substrate film through each guide roller according to a path required for vacuum aluminum plating.
In this embodiment, in step 1), the substrate film is a polyester film.
In this embodiment, in step 1), the substrate film is a PET film.
In this example, the temperature of the trap pump was controlled at-145 ℃ in step 2). Therefore, the vacuum pumping is facilitated, the workload of the collecting pump can be reduced, and the energy-saving and environment-friendly effects are achieved.
In this embodiment, in step 3), the vacuum pumping process is divided into three stages, first, a mechanical pump performs primary pumping, then a roots pump works, when the vacuum degree in the vacuum chamber reaches 10-2mbar, a diffusion pump is opened, and the high vacuum degree in the vacuum chamber, namely 10-4mbar, is further improved and maintained by the diffusion pump, so as to meet the requirement of evaporation production.
In the embodiment, the reverse side aluminum-plated VMPET film with high composite strength is further provided, and is prepared by the preparation method of the reverse side aluminum-plated VMPET film with high composite strength.
Example 4:
a preparation method of a reverse side aluminized VMPET film with high composite strength is characterized by comprising the following steps:
1) unreeling the substrate;
2) turning on the capture pump;
after the substrate film is unreeled, closing a bin body of a vacuum bin of the aluminum plating machine, opening a capture pump before vacuumizing, and condensing water in the vacuum bin of the aluminum plating machine into ice through the capture pump;
3) vacuumizing;
vacuumizing a vacuum bin of the aluminum plating machine and maintaining the vacuum degree to be 10-4 mbar;
4) heating the evaporation boat;
the time period from the start of heating the evaporation boat to normal evaporation was controlled to 14 minutes in principle. The evaporation boat is heated in 4 stages, each stage is used for 3.5 minutes, the power is respectively 20%, 45%, 60% and 75%, meanwhile, the evaporation boat is not more than 1V of voltage which is increased when being heated for the first time compared with normal heating at ordinary times, and the voltage is reduced after normal evaporation, so that the aluminum liquid spreading area of the evaporation boat can be increased, and the evaporation efficiency is improved.
5) Feeding an aluminum wire;
when the aluminum wires in the boat grooves of the evaporation boat are melted, the temperature of each boat is adjusted until the temperature of all the boats is adjusted to be within +/-0.1 ℃ (basically the same);
6) carrying out plasma treatment;
7) evaporation;
the evaporation boat is fixed on the holder for heating during evaporation; during normal production, the temperature of the evaporation boat is 1350 ℃, and simultaneously, the step 5) is carried out to continuously send the high-purity aluminum wire to the evaporation boat by the conveying motor and gasify the aluminum wire;
8) cooling;
cooling while evaporating, wherein the cooling temperature is 2 ℃;
9) measuring the thickness;
measuring a square resistance value through a continuous non-contact measurement thin film metal coating thickness system, calculating the higher or lower square resistance value according to the set square resistance value, and adjusting the thickness of the aluminum layer according to the higher or lower square resistance value in time;
10) rolling;
the rolling tension is adjusted to ensure that the film is spread flatly without edge slipping and rib breaking.
In this embodiment, in step 1), the unwinding of the substrate is to continuously unwind the substrate film through each guide roller according to a path required for vacuum aluminum plating.
In this embodiment, in step 1), the substrate film is a polyester film.
In this embodiment, in step 1), the substrate film is a PET film.
In this example, the temperature of the trap pump was controlled at-150 ℃ in step 2). Therefore, the vacuum pumping is facilitated, the workload of the collecting pump can be reduced, and the energy-saving and environment-friendly effects are achieved.
In this embodiment, in step 3), the vacuum pumping process is divided into three stages, first, a mechanical pump performs primary pumping, then a roots pump works, when the vacuum degree in the vacuum chamber reaches 10-2mbar, a diffusion pump is opened, and the high vacuum degree in the vacuum chamber, namely 10-4mbar, is further improved and maintained by the diffusion pump, so as to meet the requirement of evaporation production.
In the embodiment, in the step 6), the surface of the substrate film is treated at the running speed of 13m/s by mixing the oxygen flow of 300sccm and the argon flow of 1000sccm, controlling the current intensity to be 18A, the purity of the plasma substance to be more than 99.9% and the flow of the plasma substance to be 750sccm, so as to increase the adhesion fastness of the aluminum layer on the surface of the film.
In the embodiment, the reverse side aluminum-plated VMPET film with high composite strength is further provided, and is prepared by the preparation method of the reverse side aluminum-plated VMPET film with high composite strength.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.

Claims (9)

1. A preparation method of a reverse side aluminized VMPET film with high composite strength is characterized by comprising the following steps:
1) unreeling the substrate;
2) turning on the capture pump;
after the substrate film is unreeled, closing a bin body of a vacuum bin of the aluminum plating machine, opening a capture pump before vacuumizing, and condensing water in the vacuum bin of the aluminum plating machine into ice through the capture pump;
3) vacuumizing;
vacuumizing the vacuum chamber of the aluminum plating machine and maintaining the vacuum degree to be 10-4mbar;
4) Heating the evaporation boat;
the time for starting heating the evaporation boat to normal evaporation is controlled to be 12-16 minutes in principle. The evaporation boat is heated in 4 stages, each stage takes 3-4 minutes, the power is 0-40%, 40-50%, 50-70% and 70-80%, meanwhile, the evaporation boat is heated for the first time, the voltage is increased by no more than 1V compared with the ordinary normal heating, and the voltage is reduced after the evaporation boat is normally evaporated;
5) feeding an aluminum wire;
when the aluminum wires placed in the boat grooves of the evaporation boats are melted, the temperature of each boat is adjusted until the temperature of all the boats is adjusted to be within +/-0.1 ℃;
6) carrying out plasma treatment;
mixing oxygen flow of 200-400 sccm and argon flow of 800-1200 sccm, controlling current intensity of 15-20A, purity of plasma substance of more than 99.9% and flow of plasma substance of 500-1000 sccm, and treating the surface of the substrate film at a running speed of 12-14 m/s;
7) evaporation;
the evaporation boat is fixed on the holder for heating during evaporation; during normal production, the temperature of the evaporation boat is 1300-1400 ℃, and step 5) is carried out simultaneously to continuously send the high-purity aluminum wire to the evaporation boat by the conveying motor and gasify the aluminum wire;
8) cooling;
cooling while evaporating, wherein the cooling temperature is 0-3 ℃;
9) measuring the thickness;
measuring a square resistance value through a continuous non-contact measurement thin film metal coating thickness system, calculating the higher or lower square resistance value according to the set square resistance value, and adjusting the thickness of the aluminum layer according to the higher or lower square resistance value in time;
10) rolling;
the rolling tension is adjusted to ensure that the film is spread flatly without edge slipping and rib breaking.
2. The method for preparing the high-composite-strength back-side aluminized VMPET film according to claim 1, wherein in the step 1), the substrate is unreeled continuously by passing the substrate film through each guide roller according to a path required for vacuum aluminizing.
3. The method for preparing a high-composite-strength back-side aluminized VMPET film according to claim 2, wherein in the step 1), the base material film is a polyester film.
4. The method for preparing a high-composite-strength back-side aluminized VMPET film according to claim 2, wherein in the step 1), the base material film is a PET film.
5. The method for preparing a high composite strength reverse side aluminized VMPET film according to claim 1, wherein the temperature of the capture pump in step 2) is controlled to-150 ± 5 ℃.
6. The method for preparing a high-composite-strength back-side aluminum-plated VMPET film as claimed in claim 1, wherein in the step 3), the vacuum pumping process is divided into three stages, firstly, the mechanical pump is used for primary pumping, then, the Roots pump is used for working, when the vacuum degree in the vacuum chamber reaches 10-2mbar, the diffusion pump is opened, and the high vacuum degree in the vacuum chamber is further improved and maintained by the diffusion pump, namely 10-4mbar, so as to meet the requirement of evaporation production.
7. The method for preparing a high composite strength reverse side aluminized VMPET film according to claim 1, wherein in step 4), the evaporation boat is heated in 4 stages, each stage takes 3.5 minutes, the power is 20%, 45%, 60%, 75%, and the evaporation boat is heated for the first time to a voltage not higher than 1V than the normal heating, and the voltage is reduced after the normal evaporation.
8. The method for preparing a reverse side aluminized VMPET film with high composite strength as claimed in claim 1, wherein in step 6), the surface of the substrate film is treated at an operating speed of 13m/s by mixing an oxygen gas flow of 300sccm and an argon gas flow of 1000sccm, and controlling a current intensity of 18A and a purity of the plasma substance of more than 99.9% and a flow of the plasma substance of 750 sccm.
9. The reverse aluminum-plated VMPET film with high composite strength is characterized by being prepared by the preparation method of the reverse aluminum-plated VMPET film with high composite strength as claimed in any one of claims 1 to 8.
CN201911293306.XA 2019-12-16 2019-12-16 High-composite-strength back-side aluminum-plated VMPET film and preparation method thereof Pending CN110983259A (en)

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