CN109825806B - PET (polyethylene terephthalate) non-conductive film and preparation method thereof - Google Patents
PET (polyethylene terephthalate) non-conductive film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a PET (polyethylene terephthalate) non-conductive film and a preparation method thereof, and relates to the technical field of magnetic control coating. The technical key points are as follows: the PET non-conductive film comprises a PET film, wherein an indium tin alloy layer is magnetically sputtered on a non-hardened surface of the PET film, and a titanium pentoxide layer is magnetically sputtered on one surface, away from the PET film, of the indium tin alloy layer; the thickness of the indium tin alloy layer is less than or equal to 50 nm. According to the invention, the surface of the indium tin alloy layer is plated with the titanium pentoxide layer, so that indium and tin can be prevented from being oxidized, and the indium tin alloy layer is protected, and the indium tin alloy layer is prevented from being scratched to cause falling off; the impedance reaches more than 2000M omega, so that the application range of the non-conductive film is wider.
Description
Technical Field
The invention relates to the technical field of magnetic control coating, in particular to a PET (polyethylene terephthalate) non-conductive film and a preparation method thereof.
Background
With the vigorous development of the information age, people increasingly rely on using electronic products such as mobile phones for communication, however, most mobile phone shells are formed by plastic injection molding, the appearance is poor, further surface decoration processes such as surface spraying and non-conductive vacuum metallization are needed, and the impedance of the non-conductive film is required to be greater than or equal to 200 MOmega.
The utility model discloses a protection film for a plastic shell of a mobile phone in the Chinese utility model with the publication number CN204505999U, which is formed by superposing a bottom film layer and a metal film layer, wherein the bottom film layer is a PET layer, the thickness of the metal film layer is 180-fold and 220nm, the metal film layer is a non-conductive and metal-luster protection film formed by being sputtered on the PET layer through magnetron sputtering, the thickness of the metal film layer is 190-fold and 210nm, and the metal film layer is an indium tin alloy layer.
The protective film directly plates the indium-tin alloy layer on the surface of the PET film, and has the following defects: because the indium-tin alloy is metal, the bonding strength with PET is low, and the indium-tin alloy is easy to fall off; the surface of the indium tin alloy layer is not provided with a protective layer, so that scratch is easily caused; the foregoing two causes further cause the impedance of the protective film to be unstable.
Disclosure of Invention
In view of the defects of the prior art, an object of the present invention is to provide a PET non-conductive film having the advantages of being not easy to scratch or fall off an indium tin alloy layer, and having stable impedance.
The second purpose of the invention is to provide a preparation method of the PET non-conductive film, which has the advantages of high production effect and stable product quality.
In order to achieve the first purpose, the invention provides the following technical scheme:
the PET non-conductive film comprises a PET film, wherein an indium tin alloy layer is magnetically sputtered on a non-hardened surface of the PET film, and a titanium pentoxide layer is magnetically sputtered on one surface, away from the PET film, of the indium tin alloy layer; the thickness of the indium tin alloy layer is less than or equal to 50 nm.
By adopting the technical scheme, because the oxides of indium and tin have good conductivity, the surface of the indium-tin alloy layer is plated with the titanium pentoxide layer, and the titanium pentoxide can prevent the indium and tin from being oxidized, so that the impedance is stable; meanwhile, the function of protecting the indium tin alloy layer is achieved, and the indium tin alloy layer is prevented from being scratched to cause falling off; although indium and tin are conductive metals, when the thickness of the indium tin alloy layer is less than 50nm, the internal structure of the indium tin alloy layer is changed, and the impedance reaches more than 2000M omega, which is far higher than that of a common non-conductive film.
More preferably, the thickness of the PET film is 0.05-0.188 mm; the thickness of the indium tin alloy layer is 10-50 nm; the thickness of the titanium pentoxide layer is 10-15 nm.
By adopting the technical scheme, within the size range, the mechanical property of the PET non-conductive film can be ensured to meet the use requirement, and the impedance of the PET non-conductive film can be ensured to be more than 2000M omega.
More preferably, the mass ratio of indium to tin in the indium tin alloy layer is 3: 7.
By adopting the technical scheme, the influence of the color of the indium tin alloy layer on the light transmittance is small.
In order to achieve the second purpose, the invention provides the following technical scheme:
a preparation method of a PET non-conductive film comprises the following steps:
sending the PET film qualified by inspection into a hundred-grade dust-free workshop, tearing off a protective film on the non-hardened surface of the PET film, removing dust on the non-hardened surface of the PET film, and eliminating static electricity;
step two, winding the PET film with dust removal and static electricity removal on a winding multi-target magnetOn a cold drum of a controlled sputtering film coating machine, the hardened surface of the PET film is contacted with the cold drum, and the cold drum is vacuumized until the vacuum degree is less than 3 multiplied by 10-4Pa, introducing argon gas, and keeping the vacuum degree at 1.5 +/-0.5 multiplied by 10-1Pa；
Bombarding the non-hardened surface of the PET film by adopting an anode layer ion source, controlling the current to be 0.1-0.5A and the voltage to be 400-600V;
step four, starting the magnetron sputtering target, and depositing an indium tin alloy layer on the non-hardened surface of the PET film by adopting a direct current power supply, wherein the current of the direct current power supply is 6-8A;
and fifthly, depositing a titanium pentoxide layer on one surface of the indium tin alloy layer, which is far away from the PET film, by adopting a medium-frequency power supply, wherein the power of the medium-frequency power supply is 8-10kw, and thus obtaining the PET non-conductive film.
By adopting the technical scheme, the PET film is firstly subjected to dust removal and static elimination to prevent the PET film from adsorbing impurities, and then the anode layer ion source is adopted for bombardment, so that a rough surface is formed on the non-hardened surface of the PET film, and the bonding strength of the indium tin alloy layer and the PET film is remarkably improved; because the indium tin alloy layer and the titanium pentoxide layer are continuously deposited in the same equipment, a winding multi-target magnetron sputtering film plating machine is adopted, the production efficiency is improved, and the quality of the PET non-conductive film is stable.
More preferably, the temperature of the PET film in the third step to the fifth step is controlled to be 18-20 ℃.
By adopting the technical scheme, because the PET film can be continuously heated up when being coated, the temperature is controlled within the temperature range, the normal coating of the PET film can be ensured, and the deformation of the PET film or the uneven thickness of the coated film can be avoided.
More preferably, the temperature of the magnetron sputtering target in the third step to the fifth step is controlled to be 18-20 ℃.
By adopting the technical scheme, the magnetron sputtering target material can be continuously heated during working and is controlled within the temperature range, so that the target material is prevented from being burnt out while the target material is ensured to normally work.
More preferably, the distance between the magnetron sputtering target and the PET film is 8-15 cm.
By adopting the technical scheme, the thickness of the coating film can be controlled in the distance range.
More preferably, the linear velocity of the PET film in the third to fifth steps is 0.3 to 5 m/min.
By adopting the technical scheme, the thicker the coating film is, the lower the linear velocity of the PET film is, on the contrary, the thinner the coating film is, the higher the linear velocity of the PET film is, and under the linear velocity, the thicknesses of the indium tin alloy layer and the titanium pentoxide layer can be ensured to meet the requirements.
In summary, compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, the surface of the indium tin alloy layer is plated with the titanium pentoxide layer, and the titanium pentoxide layer can prevent indium and tin from being oxidized, so that the impedance is stable, and meanwhile, the effect of protecting the indium tin alloy layer is achieved, and the indium tin alloy layer is prevented from falling off due to scratching;
(2) although indium and tin are conductive metals, when the thickness of the indium tin alloy layer is less than 50nm, the internal structure of the indium tin alloy layer is changed, the impedance reaches more than 2000M omega and far exceeds the impedance of a common non-conductive film, so that the application range of the non-conductive film is wider;
(3) according to the invention, the anode layer ion source is adopted to bombard the non-hardened surface of the PET film before film coating, so that the non-hardened surface of the PET film forms a rough surface, the bonding strength of the indium tin alloy layer and the PET film is obviously improved, and the PET film is not easy to fall off.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1: the PET non-conductive film comprises a PET film, the light transmittance of the PET film is 90% +/-2, and the pencil hardness of the hardened surface of the PET film is less than or equal to 2H. An indium tin alloy layer is magnetically sputtered on the non-hardened surface of the PET film, a titanium pentoxide layer is magnetically sputtered on the surface of the indium tin alloy layer, which is far away from the PET film, and the titanium pentoxide layer can prevent indium and tin from being oxidized, so that the impedance of the titanium pentoxide layer is stable; meanwhile, the function of protecting the indium tin alloy layer is achieved, and the indium tin alloy layer is prevented from being scratched to cause falling off.
The thickness of the indium tin alloy layer is less than or equal to 50nm, so that the resistance of the PET non-conductive film is greater than or equal to 2000M omega. The thickness of the PET film can be 0.05-0.188mm, in this example 0.1 mm; the thickness of the indium tin alloy layer can be 10-50nm, in this embodiment 30 nm; the thickness of the titanium pentoxide layer may be 10-15nm, 12nm in this embodiment. In order to reduce the influence of the color of the indium tin alloy layer on the light transmittance, the mass ratio of indium to tin in the indium tin alloy layer is 3: 7. The PET non-conductive film can be applied to decoration of electronic product shells, protective films of touch screens and the like.
Example 2: a PET nonconductive film different from example 1 in that the thickness of the PET film was 0.05 mm; the thickness of the indium tin alloy layer is 10 nm; the thickness of the titanium pentoxide layer was 10 nm.
Example 3: a PET nonconductive film different from example 1 in that the thickness of the PET film was 0.188 mm; the thickness of the indium tin alloy layer is 50 nm; the thickness of the titanium pentoxide layer was 15 nm.
Example 4: a preparation method of a PET non-conductive film comprises the following steps:
the method comprises the following steps of firstly, carrying out appearance and performance inspection on a PET film, enabling the light transmittance of the PET film to be 90% +/-2, enabling the pencil hardness of the hardened surface of the PET film to be less than or equal to 2H, sending the PET film qualified in the appearance and performance inspection into a hundred-grade dust-free workshop, tearing off a protective film of the non-hardened surface of the PET film, carrying out dust removal on the non-hardened surface of the PET film by using a dust-sticking roller, and simultaneously eliminating static electricity by using an ion fan;
winding the dedusting and destaticizing PET film on a cold drum of a winding multi-target magnetron sputtering film plating machine, contacting the hardened surface of the PET film with the cold drum, and vacuumizing until the vacuum degree is less than 3 multiplied by 10-4Pa, introducing argon gas, and keeping the vacuum degree at 1.5 +/-0.5 multiplied by 10-1Pa；
Bombarding the non-hardened surface of the PET film by using an anode layer ion source, wherein the current is controlled to be 0.3A, and the voltage is controlled to be 500V;
fourthly, enabling the distance between the magnetron sputtering target material and the PET film to be 10cm, starting the magnetron sputtering target material, and depositing an indium tin alloy layer on the non-hardened surface of the PET film by adopting a direct current power supply, wherein the current of the direct current power supply is 7A;
and fifthly, depositing a titanium pentoxide layer on one surface of the indium tin alloy layer, which is far away from the PET film, by adopting a medium-frequency power supply, wherein the power of the medium-frequency power supply is 9kw, and thus obtaining the PET non-conductive film.
And finally, conveying the PET non-conductive film to a hundred-grade dust-free workshop, pasting a PE protective film on the surface of the titanium pentoxide layer by utilizing electrostatic adsorption, and packaging.
Wherein the temperature of the PET film in the third step to the fifth step is controlled to be 19 ℃, the temperature of the magnetron sputtering target material is controlled to be 19 ℃, and the linear speed of the PET film in the third step to the fifth step is 3 m/min.
Example 5: a PET nonconductive film, which is different from example 1 in that the third step is: and bombarding the non-hardened surface of the PET film by adopting an anode layer ion source, wherein the current is controlled to be 0.1A, and the voltage is controlled to be 400V.
Example 6: a PET nonconductive film, which is different from example 1 in that the third step is: and bombarding the non-hardened surface of the PET film by adopting an anode layer ion source, wherein the current is controlled to be 0.5A, and the voltage is controlled to be 600V.
Example 7: a PET nonconductive film is different from the PET nonconductive film in the embodiment 1 in that the current of the direct current power supply in the fourth step is 6A, and the power of the intermediate frequency power supply in the fifth step is 8 kw.
Example 8: a PET nonconductive film is different from the PET nonconductive film in the embodiment 1 in that the current of the direct current power supply in the fourth step is 8A, and the power of the intermediate frequency power supply in the fifth step is 10 kw.
Example 9: a PET non-conductive film is different from the PET non-conductive film in the embodiment 1 in that the distance between a magnetron sputtering target and the PET film is 8cm, and the linear speed of the PET film in the third step to the fifth step is 0.3 m/min.
Example 10: a PET non-conductive film is different from the PET non-conductive film in the embodiment 1 in that the distance between a magnetron sputtering target and the PET film is 15cm, and the linear speed of the PET film in the third step to the fifth step is 5 m/min.
Example 11: the difference between the PET non-conductive film and the embodiment 1 is that the temperature of the PET film is controlled to be 18 ℃ in the third step and the fifth step, and the temperature of the magnetron sputtering target is controlled to be 20 ℃.
Example 12: the difference between the PET non-conductive film and the embodiment 1 is that the temperature of the PET film is controlled to be 20 ℃ in the third step and the fifth step, and the temperature of the magnetron sputtering target is controlled to be 18 ℃.
Comparative example 1: a PET non-conductive film comprises a PET film, wherein an indium tin alloy layer is magnetically sputtered on a non-hardened surface of the PET film, and the thickness of the PET film is 0.1 mm; the thickness of the indium tin alloy layer is 30 nm.
Comparative example 2: a PET nonconductive film different from example 1 in that the indium tin alloy layer had a thickness of 80 nm.
Comparative example 3: a preparation method of a PET non-conductive film comprises the following steps:
the method comprises the following steps of firstly, carrying out appearance and performance inspection on a PET film, enabling the light transmittance of the PET film to be 90% +/-2, enabling the pencil hardness of the hardened surface of the PET film to be less than or equal to 2H, sending the PET film qualified in the appearance and performance inspection into a hundred-grade dust-free workshop, tearing off a protective film of the non-hardened surface of the PET film, carrying out dust removal on the non-hardened surface of the PET film by using a dust-sticking roller, and simultaneously eliminating static electricity by using an ion fan;
winding the dedusting and destaticizing PET film on a cold drum of a winding multi-target magnetron sputtering film plating machine, contacting the hardened surface of the PET film with the cold drum, and vacuumizing until the vacuum degree is less than 3 multiplied by 10-4Pa, introducing argon gas, and keeping the vacuum degree at 1.5 +/-0.5 multiplied by 10-1Pa；
Step three, enabling the distance between the magnetron sputtering target material and the PET film to be 10cm, starting the magnetron sputtering target material, and depositing an indium tin alloy layer on the non-hardened surface of the PET film by adopting a direct current power supply, wherein the current of the direct current power supply is 7A;
and step four, depositing a titanium pentoxide layer on one surface of the indium tin alloy layer, which is far away from the PET film, by adopting a medium-frequency power supply, wherein the power of the medium-frequency power supply is 9kw, and thus obtaining the PET non-conductive film.
And in the third step and the fourth step, controlling the temperature of the PET film to be 19 ℃, controlling the temperature of the magnetron sputtering target material to be 19 ℃, and controlling the linear speed of the PET film to be 3 m/min.
Firstly, product inspection: the non-conductive PET film of example 1 was tested for various properties and the results are shown in table 1.
Table 1 examination results of the non-conductive PET film in example 1
Second, performance test
The detection method comprises the following steps: the PET nonconductive films of examples 1 to 12 and comparative examples 1 to 3 were examined for adhesion and resistance values, respectively.
And (3) testing results and analyzing: the results of the adhesion and resistance test of the non-conductive PET films of examples 1 to 12 and comparative examples 1 to 3 are shown in table 2. As can be seen from table 2, the adhesion of examples 1 to 12 is 0 grade, the adhesion of comparative example 1 is 2 grade when no ti pentoxide layer is present, the adhesion of comparative example 3 is 4 grade when no anode layer ion source is used to bombard the non-hardened surface of the PET film before film plating, which indicates that the present invention prevents the ito layer from falling off due to scratching by plating the ti pentoxide layer on the ito layer surface; according to the invention, the anode layer ion source is adopted to bombard the non-hardened surface of the PET film before film coating, so that the non-hardened surface of the PET film forms a rough surface, the bonding strength of the indium tin alloy layer and the PET film is obviously improved, and the PET film is not easy to fall off.
The resistance values of examples 1-12 were all ≧ 2000M Ω, while comparative example 2 reduced to 0M Ω, which was conductive and not satisfactory for non-conductive films. It is shown that when the thickness of the indium tin alloy layer is only less than 50nm, the internal structure of the indium tin alloy layer is changed, the impedance reaches more than 2000M omega, which is far higher than the impedance of the common non-conductive film, so that the application range of the non-conductive film is wider.
TABLE 2 results of examination of adhesion and resistance values of the non-conductive PET films in examples 1 to 12 and comparative examples 1 to 3
| Example/comparative example numbering | Adhesion force | Resistance value |
| Example 1 | Level 0 | ≥2000MΩ |
| Example 2 | Level 0 | ≥2000MΩ |
| Example 3 | Level 0 | ≥2000MΩ |
| Example 4 | Level 0 | ≥2000MΩ |
| Example 5 | Level 0 | ≥2000MΩ |
| Example 6 | Level 0 | ≥2000MΩ |
| Example 7 | Level 0 | ≥2000MΩ |
| Example 8 | Level 0 | ≥2000MΩ |
| Example 9 | Level 0 | ≥2000MΩ |
| Example 10 | Level 0 | ≥2000MΩ |
| Example 11 | Level 0 | ≥2000MΩ |
| Example 12 | Level 0 | ≥2000MΩ |
| Comparative example 1 | Stage 2 | ≥2000MΩ |
| Comparative example 2 | Level 1 | 0MΩ |
| Comparative example 3 | 4 stage | ≥1000MΩ |
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.
Claims (8)
1. The PET non-conductive film comprises a PET film, and is characterized in that an indium tin alloy layer is magnetically sputtered on a non-hardened surface of the PET film, and a titanium pentoxide layer is magnetically sputtered on one surface, away from the PET film, of the indium tin alloy layer; the thickness of the indium tin alloy layer is less than or equal to 50 nm;
the preparation method of the PET non-conductive film comprises the following steps:
sending the PET film qualified by inspection into a hundred-grade dust-free workshop, tearing off a protective film on the non-hardened surface of the PET film, removing dust on the non-hardened surface of the PET film, and eliminating static electricity;
winding the dedusting and destaticizing PET film on a cold drum of a winding multi-target magnetron sputtering film plating machine, contacting the hardened surface of the PET film with the cold drum, and vacuumizing until the vacuum degree is less than 3 multiplied by 10-4Pa, introducing argon gas, and keeping the vacuum degree at 1.5 +/-0.5 multiplied by 10-1Pa；
Bombarding the non-hardened surface of the PET film by adopting an anode layer ion source, controlling the current to be 0.1-0.5A and the voltage to be 400-600V;
step four, starting the magnetron sputtering target, and depositing an indium tin alloy layer on the non-hardened surface of the PET film by adopting a direct current power supply, wherein the current of the direct current power supply is 6-8A;
and fifthly, depositing a titanium pentoxide layer on one surface of the indium tin alloy layer, which is far away from the PET film, by using a medium-frequency power supply, wherein the power of the medium-frequency power supply is 8-10kW, and thus obtaining the PET non-conductive film.
2. The non-conductive PET film of claim 1, wherein the PET film has a thickness of 0.05 to 0.188 mm; the thickness of the indium tin alloy layer is 10-50 nm; the thickness of the titanium pentoxide layer is 10-15 nm.
3. The PET nonconductive film of claim 1, wherein the indium-tin alloy layer has a mass ratio of indium to tin of 3: 7.
4. The PET nonconductive film of claim 1, wherein the resistance of the PET nonconductive film is equal to or greater than 2000M Ω, and the transmittance of the PET film is 90% ± 2.
5. The nonconductive PET film as set forth in claim 1, wherein the temperature of the PET film is controlled to 18-20 ℃ in the third to fifth steps of the production method.
6. The PET nonconductive film of claim 1, wherein the temperature of the magnetron sputtering target in the third to fifth steps of the preparation method is controlled to be 18-20 ℃.
7. The PET nonconductive film of claim 1, wherein the distance between the magnetron sputtering target and the PET film in the preparation method is 8-15 cm.
8. The non-conductive PET film as claimed in claim 1, wherein the linear speed of the PET film in the third to fifth steps is 0.3-5 m/min.
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