CN117966097A - Polyether-ether-ketone/Cu composite film and preparation method and application thereof - Google Patents
Polyether-ether-ketone/Cu composite film and preparation method and application thereof Download PDFInfo
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- CN117966097A CN117966097A CN202410132202.5A CN202410132202A CN117966097A CN 117966097 A CN117966097 A CN 117966097A CN 202410132202 A CN202410132202 A CN 202410132202A CN 117966097 A CN117966097 A CN 117966097A
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- 239000004696 Poly ether ether ketone Substances 0.000 title claims abstract description 84
- 229920002530 polyetherether ketone Polymers 0.000 title claims abstract description 84
- 239000002131 composite material Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 94
- 230000007704 transition Effects 0.000 claims abstract description 55
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 11
- 239000000956 alloy Substances 0.000 claims abstract description 11
- 239000010949 copper Substances 0.000 claims description 67
- 238000000034 method Methods 0.000 claims description 27
- 229910000599 Cr alloy Inorganic materials 0.000 claims description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 14
- 229910052802 copper Inorganic materials 0.000 claims description 13
- 229910018575 Al—Ti Inorganic materials 0.000 claims description 6
- QQHSIRTYSFLSRM-UHFFFAOYSA-N alumanylidynechromium Chemical compound [Al].[Cr] QQHSIRTYSFLSRM-UHFFFAOYSA-N 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 125000000524 functional group Chemical group 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 239000010408 film Substances 0.000 description 116
- 238000004544 sputter deposition Methods 0.000 description 19
- 239000000758 substrate Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 239000011521 glass Substances 0.000 description 12
- 230000007246 mechanism Effects 0.000 description 8
- 239000000523 sample Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 229920001721 polyimide Polymers 0.000 description 4
- 239000013077 target material Substances 0.000 description 4
- 239000004642 Polyimide Substances 0.000 description 3
- 238000009713 electroplating Methods 0.000 description 3
- 230000000087 stabilizing effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
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Abstract
The invention provides a polyether-ether-ketone/Cu composite film, and a preparation method and application thereof, and belongs to the technical field of copper-clad plates and current collecting films. The invention adopts high-activity Al, ti, cr or alloy thereof on the single-sided or double-sided magnetron sputtering transition layer and Cu layer of the polyether-ether-ketone film, and controls the specific types of the transition layer, thereby not only being capable of forming chemical bonds with functional groups in the polyether-ether-ketone film, but also being capable of forming metallurgical bonds with the Cu layer, thereby improving the bonding force between the polyether-ether-ketone and Cu, and the preparation method is simple, high in efficiency and free from environmental pollution. The results of the examples show that the peel strength of the composite film prepared by the invention is more than 16.76N/cm, which exceeds the requirements of the electronic industry.
Description
Technical Field
The invention relates to the technical field of copper-clad plates or current collecting films, in particular to a polyether-ether-ketone/Cu composite film, a preparation method and application thereof.
Background
In recent years, with the rapid development of 3C products, new energy automobiles and other industries, various electronic products propose a development path for lightening, thinning and multifunctionality, and higher density integration and higher bearing power of electronic circuits are required. The Flexible Copper-clad plate (Flexible Copper CLAD LAMINATE, FCCL) serving as the base material of the printed circuit board has the advantages of light weight, flexibility and the like, and is widely applied to the fields of mobile phones, flat plates, liquid crystal displays and the like at present. At the same time, the rapid development of secondary batteries requires a thinner current collecting Cu thin film (Cu foil) with higher conductivity. Whether copper-clad plates for integrated circuits or current collector films for secondary batteries, polyimide/Cu films are currently available. Because the polyether-ether-ketone has better strength and plasticity, voltage breakdown resistance and ultrathin film forming capability (PEEK film with the thickness of 3 microns can be realized in a laboratory at present) than polyimide, the polyether-ether-ketone can replace a polyimide film, and a novel PEEK/Cu film type copper-clad plate or a current collecting film for a secondary battery can be realized.
Currently, a sputtering-electroplating method is generally adopted for a composite film, namely, a Cu film is deposited on a matrix film such as polyimide through magnetron sputtering, and then the Cu film is deposited through the electroplating method, so that the composite film is thickened. The sputtering method has the advantages of high surface smoothness and capability of forming a thin-layer conductor, however, the peeling strength and the insulation reliability are slightly poor, the electroplating causes pollution to the environment, and the interface bonding force between the substrate and the Cu film is small.
According to the method, the interfacial bonding force of the Cu/organic polymer can be improved to a certain extent, but the method has the problems of higher cost, environmental pollution, low production efficiency of products and the like, and the bonding force of the prepared composite film is still relatively general. Therefore, how to improve the bonding force between the base film and Cu at low cost and high efficiency is a problem to be solved in the prior art.
Disclosure of Invention
The invention aims to provide a polyether-ether-ketone/Cu composite film, and a preparation method and application thereof. The composite film prepared by the preparation method provided by the invention has excellent binding force, and the method is simple, low in cost and high in efficiency.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a polyether-ether-ketone/Cu composite film, which comprises the following steps:
(1) Performing magnetron sputtering transition layers on one side or two sides of the polyether-ether-ketone film to obtain a polyether-ether-ketone film coated with the single-side or two-side transition layers; the transition layer comprises an Al layer, a Ti layer, a Cr layer, an Al-Ti alloy layer, an Al-Cr alloy layer, a Ti-Cr alloy layer or an Al-Ti-Cr alloy layer;
(2) And (3) coating the transition layer surface of the polyether-ether-ketone film with the single-sided or double-sided transition layer obtained in the step (1) to perform magnetron sputtering on a copper layer to obtain the polyether-ether-ketone/Cu composite film.
Preferably, the thickness of the polyether-ether-ketone film in the step (1) is 1-50 μm.
Preferably, the thickness of the transition layer in the step (1) is 2-100 nm.
Preferably, the back vacuum degree of the magnetron sputtering in the step (1) is less than 1 multiplied by 10 -3 Pa, the Ar pressure of the magnetron sputtering is 0.1-2 Pa, and the magnetron sputtering rate is 10-100 nm/min.
Preferably, the thickness of the copper layer in the step (2) is 1 to 10 μm.
Preferably, the back vacuum degree of the magnetron sputtering in the step (2) is less than 1 multiplied by 10 -3 Pa, the Ar pressure of the magnetron sputtering is 0.1-2 Pa, and the magnetron sputtering rate is 50-2000 nm/min.
Preferably, in the step (2), a bias voltage is also applied during the magnetron sputtering.
Preferably, the bias voltage is 50 to 500V.
The invention provides the polyether-ether-ketone/Cu composite film prepared by the preparation method.
The invention also provides application of the polyether-ether-ketone/Cu composite film as a flexible copper-clad plate or a secondary battery current collecting film.
The invention provides a preparation method of a polyether-ether-ketone/Cu composite film, which comprises the following steps:
(1) Performing magnetron sputtering transition layers on one side or two sides of the polyether-ether-ketone film to obtain a polyether-ether-ketone film coated with the single-side or two-side transition layers; the transition layer comprises an Al layer, a Ti layer, a Cr layer, an Al-Ti alloy layer, an Al-Cr alloy layer, a Ti-Cr alloy layer or an Al-Ti-Cr alloy layer; (2) And (3) coating the transition layer surface of the polyether-ether-ketone film with the single-sided or double-sided transition layer obtained in the step (1) to perform magnetron sputtering on a copper layer to obtain the polyether-ether-ketone/Cu composite film. The invention adopts high-activity Al, ti, cr or alloy thereof on the single-sided or double-sided magnetron sputtering transition layer and Cu layer of the polyether-ether-ketone film, and controls the specific types of the transition layer, thereby not only being capable of forming chemical bonds with functional groups in the polyether-ether-ketone film, but also being capable of forming metallurgical bonds with the Cu layer, thereby improving the bonding force between the polyether-ether-ketone and Cu, and the preparation method is simple, high in efficiency and free from environmental pollution. The results of the examples show that the peel strength of the composite film prepared by the invention is more than 16.76N/cm, which exceeds the requirements of the electronic industry.
Drawings
FIG. 1 is an XRD pattern of a composite film prepared in example 1 of the present invention;
FIG. 2 is an XRD pattern of the composite thin film prepared in example 2 of the present invention.
Detailed Description
The invention provides a preparation method of a polyether-ether-ketone/Cu composite film, which comprises the following steps:
(1) Performing magnetron sputtering transition layers on one side or two sides of the polyether-ether-ketone film to obtain a polyether-ether-ketone film coated with the single-side or two-side transition layers;
(2) And (3) coating the transition layer surface of the polyether-ether-ketone film with the single-sided or double-sided transition layer obtained in the step (1) to perform magnetron sputtering on a copper layer to obtain the polyether-ether-ketone/Cu composite film.
The magnetron sputtering transition layer is carried out on one side or two sides of the polyether-ether-ketone film, so that the polyether-ether-ketone film coated with the single side or the two sides of the transition layer is obtained.
In the present invention, the thickness of the polyetheretherketone film is preferably 1 to 50 μm. The length and the width of the polyether-ether-ketone film are not particularly limited, and the polyether-ether-ketone film can be selected according to the needs. The method can realize the preparation of the large-size composite film. When the length of the polyether-ether-ketone film is large, the invention preferably unwinds and winds simultaneously, so that continuous preparation of the large-size roll-to-roll composite film is realized, namely, the polyether-ether-ketone film is unwound on one side of the magnetron sputtering chamber, and wound on the other side of the magnetron sputtering chamber. In a preferred embodiment of the present invention, when the length of the polyetheretherketone film is large, the moving rate of the polyetheretherketone film is preferably 90 to 110mm/min.
In the present invention, the transition layer includes an Al layer, a Ti layer, a Cr layer, an Al-Ti alloy layer, an Al-Cr alloy layer, a Ti-Cr alloy layer, or an Al-Ti-Cr alloy layer. When the transition layer is an Al-Ti alloy layer, an Al-Cr alloy layer, a Ti-Cr alloy layer or an Al-Ti-Cr alloy layer, the content of each element in the alloy layer is not particularly limited, and any proportion can be used. The invention controls the types of the transition layer, adopts high-activity Al, ti, cr or alloys thereof as the transition layer, and can form chemical bonds with functional groups in the polyether-ether-ketone film and form metallurgical bonding with the Cu layer, thereby improving the bonding force between the polyether-ether-ketone and Cu.
In the present invention, the thickness of the transition layer is preferably 2 to 100nm, more preferably 5 to 50nm, and still more preferably 10 to 30nm. The present invention limits the thickness of the transition layer within the above range, and can provide the composite film with excellent bonding force.
In the present invention, the target material of the magnetron sputtering is preferably a pure Al target, a pure Ti target, a pure Cr target, an Al-Ti alloy target, an Al-Cr alloy target, a Ti-Cr alloy target or an Al-Ti-Cr alloy target. The shape of the target material is not particularly limited, and a target material having a shape well known to those skilled in the art may be used. In the present invention, the target is preferably a planar target or a cylindrical rotary target.
In the invention, the target is preferably pre-sputtered before use; the pre-sputtering time is preferably 1 to 5 minutes.
In the invention, the back vacuum degree of the magnetron sputtering is preferably less than 1 multiplied by 10 -3 Pa; the Ar pressure of the magnetron sputtering is preferably 0.1 to 2Pa, more preferably 0.2 to 1.2Pa; the magnetron sputtering rate is preferably 10 to 100nm/min, more preferably 10 to 50nm/min, and still more preferably 10 to 20nm/min. The time of the magnetron sputtering is not particularly limited, and the thickness of the transition layer is ensured to be within the range. The invention limits each parameter of the magnetron sputtering in the above range, can make the transition layer more uniform, better combine with the polyether-ether-ketone film, and further improve the combination force of the composite film.
The present invention preferably controls the magnetron sputtering power to control the magnetron sputtering rate. The invention preferably comprises the steps of firstly fixing magnetron sputtering power to 200W, sputtering for 5min on a glass substrate, then increasing the power to 500W, stabilizing for 2min, sputtering for 5min on another glass substrate, increasing the power by 300W each time, respectively sputtering for 5min on different glass substrates until the power is increased to 10kW, taking out the glass substrates, measuring the thickness of a sputtered film by using a step meter, and obtaining the quantitative relation between the sputtering power and the sputtering rate.
After the polyether-ether-ketone film coated by the single-sided or double-sided transition layer is obtained, the magnetron sputtering copper layer is performed on the surface of the transition layer of the polyether-ether-ketone film coated by the single-sided or double-sided transition layer, so that the polyether-ether-ketone/Cu composite film is obtained.
In the present invention, the thickness of the copper layer is preferably 1 to 10 μm.
In the invention, the target material of the magnetron sputtering is preferably a pure Cu target.
In the invention, the back vacuum degree of the magnetron sputtering is preferably less than 1 multiplied by 10 -3 Pa; the Ar pressure of the magnetron sputtering is preferably 0.1 to 2Pa, more preferably 0.2 to 1.2Pa; the magnetron sputtering rate is preferably 50 to 2000nm/min,100 to 1000nm/min, and more preferably 200 to 300nm/min. In the present invention, it is also preferable to apply a bias voltage at the time of the magnetron sputtering; the bias voltage is preferably 50 to 500V. In the invention, the bias voltage can realize control of the texture of the Cu layer (111), which is beneficial to improving the conductivity of the composite film. The time of the magnetron sputtering is not particularly limited, and the thickness of the copper layer is ensured to be within the range. The invention limits each parameter of the magnetron sputtering in the above range, can make the copper layer more uniform, and realizes metallurgical bonding with the transition layer, thereby further improving the bonding force of the composite film.
The invention adopts high-activity Al, ti, cr or alloy thereof on the single-sided or double-sided magnetron sputtering transition layer and Cu layer of the polyether-ether-ketone film, and controls the specific types of the transition layer, thereby not only being capable of forming chemical bonds with functional groups in the polyether-ether-ketone film, but also being capable of forming metallurgical bonds with the Cu layer, thereby improving the bonding force between the polyether-ether-ketone and Cu, simultaneously being capable of realizing the preparation of large-size composite film, and having simple preparation method, low cost, high efficiency and no environmental pollution.
The invention provides the polyether-ether-ketone/Cu composite film prepared by the preparation method.
The composite film prepared by the invention has excellent binding force, and the thickness can be adjusted according to the requirement.
The invention also provides application of the polyether-ether-ketone/Cu composite film as a flexible copper-clad plate or a secondary battery current collecting film.
The operation of the application is not particularly limited, and the application technical scheme well known to those skilled in the art can be adopted.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
(1) And installing a pure Al target and a pure Cu target in the magnetron sputtering chamber, and installing a series of glass substrates on a continuous sample rack for testing the quantitative relation between magnetron sputtering power and sputtering rate. When the vacuum degree of the magnetron sputtering chamber reaches 3X 10 -4 Pa, high-purity Ar gas is filled, in the whole magnetron sputtering process, the flowing Ar gas pressure is 0.5Pa, an Al target is started to perform pre-sputtering for 3 minutes, the sputtering power is fixed at 200W, then an Al film is subjected to magnetron sputtering on a glass substrate, and the sputtering time is 5 minutes; continuously increasing the Al magnetron sputtering power to 500W, stabilizing for 2 minutes, continuously moving the next glass substrate, and performing magnetron sputtering for 5 minutes; in the same way, the magnetron sputtering power of the Al target is increased to 10kW. Taking out the glass substrate, measuring the thickness of the Al film by using a step instrument, and obtaining a series of quantitative relations between magnetron sputtering power and the magnetron sputtering rate of Al;
By the same method, a series of Cu films under different powers are subjected to magnetron sputtering, and a quantitative relation between the magnetron sputtering power of a Cu target and the magnetron sputtering rate of Cu is constructed.
(2) Loading a roll of polyether-ether-ketone film (with the thickness of 0.015 mm) into an unreeling device of a magnetron sputtering chamber, fixing the polyether-ether-ketone film on a reeling mechanism at the other side, vacuumizing the whole magnetron sputtering device, when the vacuum degree reaches 3X 10 -4 Pa, filling high-purity Ar gas, starting an Al target to perform pre-sputtering for 3 minutes in the whole magnetron sputtering process when the flowing Ar gas pressure is 0.5Pa, starting the unreeling and reeling mechanism to enable the polyether-ether-ketone film to run in the magnetron sputtering chamber, fixing the magnetron sputtering rate of an Al target to be 20nm/min, enabling the moving rate of the polyether-ether-ketone film to be 100mm/min, and performing magnetron sputtering on one side of the polyether-ether-ketone film to obtain the polyether-ether-ketone film coated by an Al transition layer with the thickness of 15 nm;
(3) And loading the polyether-ether-ketone film coated by the Al transition layer into an unreeling device of a magnetron sputtering chamber, fixing the polyether-ether-ketone film on a reeling mechanism at the other side, vacuumizing the whole magnetron sputtering device, filling high-purity Ar gas when the vacuum degree is 3×10 -4 Pa, starting a Cu target to perform pre-sputtering for 3 minutes in the whole magnetron sputtering process, and starting the unreeling and reeling mechanism to enable the polyether-ether-ketone film to run in the magnetron sputtering chamber, wherein the magnetron sputtering rate of a fixed Cu target is 300nm/min, and the moving rate of the polyether-ether-ketone film is 100mm/min, so that a Cu layer with the thickness of 1.0 mu m is obtained.
The XRD pattern of the composite film prepared in example 1 is shown in FIG. 1. It can be seen from fig. 1 that the surface of the composite film is entirely composed of copper and has no diffraction peak of the transition layer metal Al, which means that the transition layer Al has an excellent ability to couple the polyetheretherketone film with the Cu layer.
The internal resistivity of the composite film prepared in example 1 was measured by the four-probe resistance method and found to be 3.9. Mu. Ohm. Cm, which is lower than the square resistivity of Cu of the same thickness in the current market by 5 to 8. Mu. Ohm. Cm.
The composite film prepared in example 1 was tested according to GB/T13557-2017 for peel strength of 16.67N/cm, exceeding the electronic industry requirements.
Example 2
(1) And installing a pure Ti target and a pure Cu target in the magnetron sputtering chamber, and installing a series of glass substrates on a continuous sample rack for testing the quantitative relation between magnetron sputtering power and sputtering rate. When the vacuum degree of the magnetron sputtering chamber reaches 3X 10 -4 Pa, high-purity Ar gas is filled, in the whole magnetron sputtering process, the flowing Ar gas pressure is 0.8Pa, a Ti target is started to perform pre-sputtering for 3 minutes, the sputtering power is fixed at 200W, then a Ti film is subjected to magnetron sputtering on a glass substrate, and the sputtering time is 5 minutes; continuously increasing the Ti magnetron sputtering power to 500W, stabilizing for 2 minutes, continuously moving the next glass substrate, and performing magnetron sputtering for 5 minutes; in the same way, the magnetron sputtering power of the Ti target is increased to 10kW. Taking out the glass substrate, measuring the thickness of the Ti film by using a step instrument, and obtaining a series of quantitative relations between the magnetron sputtering power and the magnetron sputtering rate of Ti;
By the same method, a series of Cu films under different powers are subjected to magnetron sputtering, and a quantitative relation between the magnetron sputtering power of a Cu target and the magnetron sputtering rate of Cu is constructed.
(2) Loading a roll of polyether-ether-ketone film (with the thickness of 0.05 mm) into an unreeling device of a magnetron sputtering chamber, fixing the polyether-ether-ketone film on a reeling mechanism at the other side, vacuumizing the whole magnetron sputtering device, when the vacuum degree reaches 3X 10 -4 Pa, filling high-purity Ar gas, starting a Ti target to perform pre-sputtering for 3 minutes when the flowing Ar gas pressure is 0.8Pa in the whole magnetron sputtering process, starting the unreeling and reeling mechanism to enable the polyether-ether-ketone film to run in the magnetron sputtering chamber, fixing the magnetron sputtering rate of a Ti target to be 10nm/min, enabling the moving rate of the polyether-ether-ketone film to be 100mm/min, and performing magnetron sputtering on one side of the polyether-ether-ketone film to obtain the polyether-ether-ketone film coated by a Ti transition layer with the thickness of 15 nm;
(3) And loading the polyether-ether-ketone film coated by the Ti transition layer into an unreeling device of a magnetron sputtering chamber, fixing the polyether-ether-ketone film on a reeling mechanism at the other side, vacuumizing the whole magnetron sputtering device, filling high-purity Ar gas when the vacuum degree is 3×10 -4 Pa, starting a Cu target to perform pre-sputtering for 3 minutes in the whole magnetron sputtering process, starting the unreeling and reeling mechanism to enable the polyether-ether-ketone film to run in the magnetron sputtering chamber, wherein the magnetron sputtering rate of a fixed Cu target is 200nm/min, the bias voltage is 150V, and the moving rate of the polyether-ether-ketone film is 100mm/min, so that a Cu layer with the thickness of 1.5 mu m is obtained.
The XRD pattern of the composite film prepared in example 2 is shown in FIG. 2. It can be seen from fig. 2 that the surface of the composite film is entirely composed of copper and has no diffraction peak of the transition layer metal Ti, which means that the transition layer Ti has an excellent ability to couple the polyetheretherketone film with the Cu layer.
The internal resistivity of the composite film prepared in example 2 was measured by the four-probe resistance method, and as a result, it was 2.8. Mu. Ohm. Cm, which is lower than the square resistivity of Cu of the same thickness in the current market by 5 to 8. Mu. Ohm. Cm.
The peel strength value of the composite film prepared in example 2 was 17.24N/cm, tested according to GB/T13557-2017, exceeding the electronic industry requirements.
Comparative example 1
The transition layer in example 1 was replaced with Fe, and the other parameters were the same as in example 1.
The internal resistivity of the composite film prepared in comparative example 1 was measured by a four-probe resistance method, and found to be 4.3. Mu. Ω. Cm.
The peel strength value of the composite film prepared in accordance with comparative example 1 was 8.62N/cm as measured in accordance with GB/T13557-2017.
Comparative example 2
The transition layer in example 1 was replaced with Ni, and the other parameters were the same as in example 1.
The internal resistivity of the composite film prepared in comparative example 2 was measured by a four-probe resistance method, and found to be 4.0. Mu. Ω. Cm.
The peel strength value of the composite film prepared in accordance with comparative example 2 was 10.35N/cm as measured in accordance with GB/T13557-2017.
Comparative example 3
The transition layer in example 1 was replaced with Mg, and the other parameters were the same as in example 1.
The internal resistivity of the composite film prepared in comparative example 3 was measured by a four-probe resistance method, and found to be 4.6. Mu. Ω. Cm.
The peel strength value of the composite film prepared in comparative example 3 was 6.24N/cm according to GB/T13557-2017 test.
Comparative example 4
The transition layer in example 1 was omitted and the other parameters were the same as in example 1.
The internal resistivity of the composite film prepared in comparative example 4 was measured by a four-probe resistance method, and found to be 4.1. Mu. Ω. Cm.
The peel strength value of the composite film prepared in accordance with comparative example 4 was 3.63N/cm as measured in accordance with GB/T13557-2017.
In conclusion, the invention magnetron sputters the transition layer on the surface of the polyether-ether-ketone film, controls the types of the transition layer and improves the binding force of the composite film.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. A preparation method of a polyether-ether-ketone/Cu composite film comprises the following steps:
(1) Performing magnetron sputtering transition layers on one side or two sides of the polyether-ether-ketone film to obtain a polyether-ether-ketone film coated with the single-side or two-side transition layers; the transition layer comprises an Al layer, a Ti layer, a Cr layer, an Al-Ti alloy layer, an Al-Cr alloy layer, a Ti-Cr alloy layer or an Al-Ti-Cr alloy layer;
(2) And (3) coating the transition layer surface of the polyether-ether-ketone film with the single-sided or double-sided transition layer obtained in the step (1) to perform magnetron sputtering on a copper layer to obtain the polyether-ether-ketone/Cu composite film.
2. The method according to claim 1, wherein the polyether-ether-ketone film in the step (1) has a thickness of 1 to 50. Mu.m.
3. The method according to claim 1, wherein the thickness of the transition layer in the step (1) is 2 to 100nm.
4. The method according to claim 1, wherein the back vacuum degree of the magnetron sputtering in the step (1) is less than 1×10 -3 Pa, the Ar pressure of the magnetron sputtering is 0.1-2 Pa, and the magnetron sputtering rate is 10-100 nm/min.
5. The method according to claim 1, wherein the copper layer in the step (2) has a thickness of 1 to 10 μm.
6. The method according to claim 1, wherein the back vacuum degree of the magnetron sputtering in the step (2) is less than 1×10 -3 Pa, the Ar pressure of the magnetron sputtering is 0.1-2 Pa, and the magnetron sputtering rate is 50-2000 nm/min.
7. The method of claim 6, wherein the step (2) is performed by magnetron sputtering while applying a bias voltage.
8. The method of claim 7, wherein the bias voltage is 50-500V.
9. The polyether-ether-ketone/Cu composite film prepared by the preparation method of any one of claims 1 to 8.
10. The use of the polyetheretherketone/Cu composite film of claim 9 as a flexible copper-clad plate or a secondary battery current collector.
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