CN111278231B - Flexible transfer printing method of laser-induced carbon-based electronic element - Google Patents
Flexible transfer printing method of laser-induced carbon-based electronic element Download PDFInfo
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- CN111278231B CN111278231B CN202010096514.7A CN202010096514A CN111278231B CN 111278231 B CN111278231 B CN 111278231B CN 202010096514 A CN202010096514 A CN 202010096514A CN 111278231 B CN111278231 B CN 111278231B
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- based electronic
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/105—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern by conversion of non-conductive material on or in the support into conductive material, e.g. by using an energy beam
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/20—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern by affixing prefabricated conductor pattern
Abstract
Provides a laser inductionA method of flexible transfer printing of carbon-based electronic components, comprising the steps of: the preparation method comprises the following steps: combining a sacrificial layer on the hard substrate, and combining a photosensitive polyimide film on the sacrificial layer; an induction step: by using CO2Laser-induced carbonization of a photosensitive polyimide film to form a carbon-based electronic component; a transfer printing step: transferring a carbon-based electronic element and a photosensitive polyimide film that is not carbonized to a flexible substrate; an exposure step: exposing the carbon-based electronic element and the non-carbonized photosensitive polyimide film to ultraviolet light; a clearing step: cleaning the non-carbonized photosensitive polyimide film irradiated by ultraviolet light by using a cleaning agent; the bonding force between the sacrificial layer and the photosensitive polyimide film and the carbon-based electronic element is smaller than that between the photosensitive polyimide film and the flexible substrate. The non-carbonized polyimide film can be dissolved in a cleaning agent and washed away, thereby obtaining a carbon-based electronic component that cannot be dissolved by the cleaning agent.
Description
Technical Field
The invention relates to the field of flexible stretchable electronic devices, in particular to a flexible transfer printing method of a laser-induced carbon-based electronic element.
Background
With the rapid development of the modern electronics industry and large-scale consumer market, the manufacture and application of flexible electronic devices has become the leading edge of modern electronics research. Generally, in the manufacture of flexible conductive patterns such as electrodes and circuits, a metal layer is spin-coated on a polyimide film, then photolithography is performed with the aid of a mask plate, and then metal wires grown on the polyimide film are transferred to a flexible stretchable substrate (e.g., a substrate made of polydimethylsiloxane, silicone rubber, aliphatic aromatic random copolyester, etc.), and then excess polyimide film is removed by reactive ion etching.
In view of the limitation of the use of a mask plate, a method of directly inducing carbonization of polyimide by laser to directly form an electrode or a circuit on a polyimide film has been proposed in the present stage. Laser-induced polyimide carbonization forms graphene circuits or electrodes that are in bulk rather than a homogenous material like metal electrodes or wires. The graphene electrode or circuit bulges out of the polyimide film, and the bonding force between the stamp for transfer printing and the graphene electrode or circuit is smaller than the bonding force between the graphene electrode or circuit and the non-carbonized polyimide.
The following problems exist when transferring graphene electrodes or circuits onto flexible substrates: the graphene electrode or the circuit is not easily separated from the polyimide film, and a transfer failure is easily caused, that is, only a part of the graphene electrode and the circuit is transferred, and the other part is left in the polyimide film.
Disclosure of Invention
The present invention has been made in view of the state of the art described above. The invention aims to provide a flexible transfer printing method of a laser-induced carbon-based electronic element, which can obtain a better transfer printing effect in the aspect of transferring the carbon-based electronic element.
The flexible transfer printing method of the laser-induced carbon-based electronic element comprises the following steps:
the preparation method comprises the following steps: combining a sacrificial layer on a hard substrate, and combining a photosensitive polyimide film on the sacrificial layer;
an induction step: by using CO2Laser-induced carbonization of the photosensitive polyimide film to form a carbon-based electronic component;
a transfer printing step: transferring the carbon-based electronic elements and the photosensitive polyimide film that is not carbonized to a flexible substrate;
an exposure step: exposing the carbon-based electronic element and the photosensitive polyimide film that is not carbonized to ultraviolet light;
a clearing step: cleaning the non-carbonized photosensitive polyimide film irradiated by the ultraviolet light with a cleaning agent;
the bonding force between the sacrificial layer and the photosensitive polyimide film and between the sacrificial layer and the carbon-based electronic element is smaller than the bonding force between the photosensitive polyimide film and between the carbon-based electronic element and the flexible substrate.
Preferably, the exposure step includes a first exposure step and a second exposure step, the removal step includes a first removal step and a second removal step, and the induction step, the first exposure step, the first removal step, the transfer step, the second exposure step, and the second removal step are performed in this order;
after the first exposure step and the first removal step, the photosensitive polyimide film on the side of the carbon-based electronic element is removed;
after the second exposure step and the second removal step, the photosensitive polyimide film between the carbon-based electronic element and the sacrificial layer is removed.
Preferably, in the first removing step, the carbon-based electronic element and the photosensitive polyimide film are immersed in the cleaning agent.
Preferably, the transfer step is followed by the exposure step in which the carbon-based electronic element and the photosensitive polyimide film that is not carbonized are subjected to one exposure.
Preferably, the photosensitive polyimide film has a thickness greater than that of the sacrificial layer.
Preferably, the wavelength of the ultraviolet light is 355 nm.
Preferably, in the preparation step, a photosensitive polyimide in a liquid state is spin-coated on the sacrificial layer, and then the temperature is raised stepwise to dry the photosensitive polyimide in a liquid state at a plurality of different temperatures.
Preferably, the carbon-based electronic element comprises a graphene electrode and/or a graphene circuit.
Preferably, the material of the sacrificial layer comprises polymethyl methacrylate, and the material of the flexible substrate comprises polydimethylsiloxane and/or aliphatic aromatic random copolyester.
Preferably, in the inducing step, the CO is emitted2Prior to the laser, a desired processing pattern is input into the laser processing platform such that the laser-induced carbon-based electronic component (31) forms a conductive pattern having the pattern.
The technical scheme provided by the disclosure at least has the following beneficial effects:
upon exposure to ultraviolet light, the non-carbonized polyimide film chemically reacts to become soluble in a cleaning agent such as acetone, while in CO2The polyimide film carbonized by the photothermal reaction under laser cannot be washed away by the cleaning agent. After the exposure step, the non-carbonized polyimide film is cleaned by a cleaning agent to obtain the required carbon-based electronic element.
Drawings
FIG. 1 is a schematic diagram of the operational steps of one embodiment of a method of laser-induced flexible transfer of carbon-based electronic components provided by the present disclosure.
Fig. 2 is a schematic diagram of the operational steps of another embodiment of a method of laser-induced flexible transfer of carbon-based electronic elements provided by the present disclosure.
Description of reference numerals:
1 hard substrate, 2 sacrificial layers, 31 laser-induced carbon-based electronic elements, 32 photosensitive polyimide film, 4 flexible substrate and 5 ultraviolet light.
Detailed Description
Exemplary embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood that the detailed description is intended only to teach one skilled in the art how to practice the invention, and is not intended to be exhaustive or to limit the scope of the invention.
The present disclosure provides a flexible transfer method of laser-induced carbon-based electronic elements 31 for transferring laser-induced carbon-based electronic elements 31 to a flexible substrate 4.
As shown in fig. 1, in one embodiment, the flexible transfer method includes sequentially:
the preparation method comprises the following steps: bonding a sacrificial layer 2 (such as polymethyl methacrylate) on a hard substrate 1 (such as a silicon wafer, a glass plate, etc.), and bonding a photosensitive polyimide film 32 on the sacrificial layer 2;
an induction step: by using CO2Laser-induced photosensitive polyimide film32 to form carbon-based electronic component 31;
a transfer printing step: transferring the carbon-based electronic element 31 and the non-carbonized photosensitive polyimide film 32 to the flexible substrate 4 (e.g., polydimethylsiloxane, aliphatic aromatic random copolyester, etc.);
an exposure step: exposing the carbon-based electronic element 31 and the photosensitive polyimide film 32 that is not carbonized to ultraviolet light 5;
a clearing step: the non-carbonized photosensitive polyimide film 32 irradiated with the ultraviolet light 5 is cleaned with a cleaning agent (e.g., acetone or the like).
The side of the carbon-based electronic element 31 facing the hard substrate 1 is the lower side, and the side facing the flexible substrate 4 is the upper side, as defined below. It should be understood that the upper and lower sides herein are defined only for the purpose of convenience of description, and do not necessarily correspond to the upper and lower sides in the space at the time of actual production.
CO emission using, for example, a laser machining platform2Laser, CO2The laser rapidly carbonizes the surface of the photosensitive polyimide film 32 directly into a carbon-based electronic component 31, such as a graphene circuit or electrode. In the emission of CO2Prior to the laser, a desired processing pattern can be input into the laser processing platform, so that the carbon-based electronic component 31 can be formed into a designed (having the desired processing pattern) conductive pattern on the photosensitive polyimide film 32 by using a laser-induced technique.
The bonding force between the sacrificial layer 2 and the photosensitive polyimide film 32 and the laser-induced carbon-based electronic element 31 is smaller than the bonding force between the photosensitive polyimide film 32 and the laser-induced carbon-based electronic element 31 and the flexible substrate 4, so that in the transfer step, a weak bonding force interface is formed between the photosensitive polyimide film 32 and the carbon-based electronic element 31 and the sacrificial layer 2, a strong bonding force interface is formed between the photosensitive polyimide film 32 and the carbon-based electronic element 31 and the flexible substrate 4, and the photosensitive polyimide film 32 and the carbon-based electronic element 31 can be detached from the sacrificial layer 2 and bonded to the flexible substrate 4.
When exposed to ultraviolet light 5, the non-carbonized photosensitive polyimide film 32 chemically reacts to become soluble in a cleaning agent such as acetone in CO2Under laserThe photosensitive polyimide film 32 (which has been formed into the carbon-based electronic element 31) carbonized by the photothermal reaction cannot be washed away by the cleaning agent. After the exposure step, the photosensitive polyimide film 32 that has not been carbonized is cleaned with a cleaning agent to obtain the desired carbon-based electronic component 31.
In this embodiment, the carbon-based electronic element 31 and the unexposed photosensitive polyimide film 32 are exposed once, and then removed after exposure, and the whole of the photosensitive polyimide film 32 that is not carbonized can be removed by one exposure and one removal, and the process is simple.
In another embodiment, as shown in fig. 2, the flexible transfer method includes the above steps, and the exposure step includes a first exposure step and a second exposure step performed before and after the transfer step, respectively, and the cleaning step includes a first cleaning step and a second cleaning step performed after the first exposure step and the second exposure step, respectively. Specifically, the steps are performed in the following order: the method comprises a preparation step, an induction step, a first exposure step, a first cleaning step, a transfer printing step, a second exposure step and a second cleaning step.
After the induction step, it is possible that only a portion of the thickness of the photosensitive polyimide film 32 can be carbonized to form the carbon-based electronic element 31, while the photosensitive polyimide film 32 that is not carbonized is still present on the lower surface of the carbon-based electronic element 31, i.e., between the carbon-based electronic element 31 and the sacrificial layer 2.
In the first exposure step, the upper surface of the carbon-based electronic component 31 may be irradiated with ultraviolet light 5, and in the second exposure step, the lower surface of the photosensitive polyimide film 32 that is not carbonized may be irradiated with ultraviolet light 5. The carbon-based electronic component 31 and the non-carbonized photosensitive polyimide film 32 may be soaked in a cleaning agent in the first cleaning step, thereby cleaning the non-carbonized photosensitive polyimide film 32.
The first exposure step and the first cleaning step may be used to remove the photosensitive polyimide film 32 that is not carbonized on the side (perpendicular to the up-down direction) of the carbon-based electronic component 31. A second exposure step and a second cleaning step may be used to remove the non-carbonized photosensitive polyimide film 32 that may be present between the carbon-based electronic element 31 and the sacrificial layer 2.
In the flexible transfer printing method provided by the present disclosure, the wavelength of the ultraviolet light 5 used is 10nm to 380nm, and preferably, deep ultraviolet light having a wavelength of about 355nm is used.
The photosensitive polyimide film 32 may have a thickness greater than that of the sacrificial layer 2, and the carbon-based electronic component 31 is formed to protrude from the upper surface of the photosensitive polyimide film 32.
Carbon-based electronic component 31 may be an electronic component made of: single-layer graphene, multi-layer graphene, carbon fibers, carbon tubes (i.e., laser-induced graphene material).
The liquid photosensitive polyimide may be spin-coated on the sacrificial layer 2 and then heated in steps to dry the liquid photosensitive polyimide at a plurality of different temperatures to form a polyimide film. The polyimide film is relatively flat and is not easy to form bubbles inside.
The above-described other embodiment is described in detail below.
The preparation method comprises the following steps:
1. with N2Blowing clean 4 inches of the surface of the silicon wafer, and spin-coating liquid polymethyl methacrylate on the surface of the silicon wafer at a speed of 600rpm for 6s and a speed of 3000rpm for 30 s;
2. heating the heating table to 180 ℃ and curing the polymethyl methacrylate for 20 minutes;
3. spin coating a liquid photosensitive polyimide on the polymethylmethacrylate-plated silicon wafer at a speed of 800rpm for 8s and a speed of 1000rpm for 30 s;
4. the liquid photosensitive polyimide was baked in an oven in a stepwise heating manner of 60 ℃ for 2 hours, 80 ℃ for 2 hours, 100 ℃ for 2 hours, 120 ℃ for 2 hours, 150 ℃ for 2 hours, 180 ℃ for 2 hours, and 200 ℃ for 2 hours in this order.
An induction step:
the figure of the electrode is designed by CAD in advance and is arranged on a general laser processing platform so as to lead the electrode to be arranged on the general laser processing platformWith CO2The laser induces graphene electrodes on the photosensitive polyimide film 32.
A first exposure step:
the graphene electrode and the surface of the photosensitive polyimide film 32 were irradiated with deep ultraviolet light (wavelength 355nm) from a photolithography machine for 10 seconds.
A first clearing step:
1. repeatedly soaking a sample on a silicon wafer in acetone, washing off the non-carbonized photosensitive polyimide film 32 by using the acetone, and only leaving a graphene electrode;
2. the non-carbonized photosensitive polyimide film 32 is cleaned, and the electrode on the silicon wafer is dried, so that the acetone is easy to volatilize, and the silicon wafer is dried in a fume hood at normal temperature for 2 hours;
3. with N2And further drying the surface of the graphene electrode.
A transfer printing step:
1. and (3) attaching the polydimethylsiloxane film to the upper surface of the laser-induced graphene electrode, and then pulling up the polydimethylsiloxane film from the polymethyl methacrylate at a high speed, so that the laser-induced graphene electrode can be completely transferred to the polydimethylsiloxane film.
A second exposure step:
a small amount of the non-carbonized photosensitive polyimide film 32 may remain on the lower surface of the laser-induced graphene electrode, and is exposed to deep ultraviolet light for 10 seconds.
A second clearing step:
1. washing the non-carbonized photosensitive polyimide film 32 with acetone;
2. the acetone washed laser-induced graphene electrode was dried in a fume hood at room temperature.
It should be understood that the above embodiments are only exemplary and are not intended to limit the present invention. Various modifications and changes may be made to the embodiments in the art without departing from the scope of the invention.
Claims (9)
1. A flexible transfer printing method of a laser-induced carbon-based electronic element is characterized by comprising the following steps:
the preparation method comprises the following steps: bonding a sacrificial layer (2) on a hard substrate (1), and bonding a photosensitive polyimide film (32) on the sacrificial layer (2);
an induction step: by using CO2Laser-induced carbonization of the photosensitive polyimide film (32) to form a carbon-based electronic element (31), the carbon-based electronic element (31) comprising a graphene electrode and/or a graphene circuit;
a transfer printing step: transferring the carbon-based electronic elements (31) and the photosensitive polyimide film (32) that is not carbonized to a flexible substrate (4);
an exposure step: exposing the carbon-based electronic elements (31) and the photosensitive polyimide film (32) that is not carbonized to ultraviolet light (5);
a clearing step: cleaning the non-carbonized photosensitive polyimide film (32) irradiated with the ultraviolet light (5) with a cleaning agent;
the bonding force between the sacrificial layer (2) and the photosensitive polyimide film (32) and the carbon-based electronic element (31) is smaller than the bonding force between the photosensitive polyimide film (32) and the carbon-based electronic element (31) and the flexible substrate (4).
2. The method of claim 1, wherein the flexible transfer printing of the laser-induced carbon-based electronic component comprises:
the exposure step includes a first exposure step and a second exposure step, the removal step includes a first removal step and a second removal step, and the induction step, the first exposure step, the first removal step, the transfer step, the second exposure step, and the second removal step are performed in order;
after the first exposure step and the first removal step, the photosensitive polyimide film (32) on the side of the carbon-based electronic element (31) is removed;
after the second exposure step and the second removal step, the photosensitive polyimide film (32) between the carbon-based electronic element (31) and the sacrificial layer (2) is removed.
3. The method of claim 2, wherein in the first removing step, the carbon-based electronic component (31) and the photosensitive polyimide film (32) are immersed in the cleaning agent.
4. The method for laser-induced flexible transfer of carbon-based electronic components according to claim 1, wherein the transfer step is followed by the exposure step in which the carbon-based electronic components (31) and the photosensitive polyimide film (32) that is not carbonized are exposed once.
5. The method of claim 1, wherein the photosensitive polyimide film (32) has a thickness greater than the thickness of the sacrificial layer (2).
6. The method of claim 1, wherein the ultraviolet light (5) has a wavelength of 355 nm.
7. The method of claim 1, wherein in the preparing step, a photosensitive polyimide in a liquid state is spin-coated on the sacrificial layer (2), and then the temperature is raised stepwise to dry the photosensitive polyimide in a liquid state at a plurality of different temperatures.
8. The method of claim 1, wherein the material of the sacrificial layer (2) comprises polymethyl methacrylate and the material of the flexible substrate (4) comprises polydimethylsiloxane and/or aliphatic aromatic random copolyester.
9. The method of claim 1, wherein in the inducing step, the carbon-based electronic component is irradiatedInjecting the CO2Prior to the laser, a desired processing pattern is input into the laser processing platform such that the laser-induced carbon-based electronic component (31) forms a conductive pattern having the pattern.
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| EP0891877A2 (en) * | 1997-07-14 | 1999-01-20 | E.I. Du Pont De Nemours And Company | Laser-induced thermal transfer recording process |
| WO2002074027A1 (en) * | 2001-03-12 | 2002-09-19 | Agency For Science, Technology And Research | Improved laser metallisation circuit formation and circuits formed thereby |
| CN107039257A (en) * | 2017-04-06 | 2017-08-11 | 清华大学深圳研究生院 | A kind of graphical preparation method of induced with laser graphene and extent product |
| CN108243575A (en) * | 2016-12-27 | 2018-07-03 | Bgt材料有限公司 | The manufacturing method of polymeric printing circuit board |
| CN110392489A (en) * | 2019-07-09 | 2019-10-29 | 江苏大学 | A kind of preparation method of the deformable wiring board based on shape-memory polymer |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8056222B2 (en) * | 2008-02-20 | 2011-11-15 | The United States Of America, As Represented By The Secretary Of The Navy | Laser-based technique for the transfer and embedding of electronic components and devices |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0891877A2 (en) * | 1997-07-14 | 1999-01-20 | E.I. Du Pont De Nemours And Company | Laser-induced thermal transfer recording process |
| WO2002074027A1 (en) * | 2001-03-12 | 2002-09-19 | Agency For Science, Technology And Research | Improved laser metallisation circuit formation and circuits formed thereby |
| CN108243575A (en) * | 2016-12-27 | 2018-07-03 | Bgt材料有限公司 | The manufacturing method of polymeric printing circuit board |
| CN107039257A (en) * | 2017-04-06 | 2017-08-11 | 清华大学深圳研究生院 | A kind of graphical preparation method of induced with laser graphene and extent product |
| CN110392489A (en) * | 2019-07-09 | 2019-10-29 | 江苏大学 | A kind of preparation method of the deformable wiring board based on shape-memory polymer |
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