CN115805367A - Metal nanowire impact welding device and method based on laser thermal coupling effect - Google Patents
Metal nanowire impact welding device and method based on laser thermal coupling effect Download PDFInfo
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Abstract
The invention discloses a metal nanowire impact welding device and method based on laser thermal coupling effect, comprising a laser, a metal nanowire and an online monitoring system; the positive pulse laser beam impacts the metal nanowire; simultaneously, reversely heating the laser beam to heat the metal nanowires; the upper part of the metal nanowire is sequentially provided with a restraint layer, an absorption layer and a protective layer from top to bottom, and the lower part of the metal nanowire is provided with the restraint layer; the online monitoring system is used for monitoring the welding condition of the metal nanowires in real time. The method effectively heats the metal nanowire node area through the plasmon, impacts the nanowires by means of the pulse laser, shortens the distance between adjacent nanowires, reduces the virtual lapping phenomenon, strengthens the heating effect, can realize high-reliability welding operation of the spatially staggered nanowires under the condition that the metal nanowires are not melted integrally, and is a novel metal nanowire welding method with high feasibility and wide application range.
Description
Technical Field
The invention relates to the technical field of welding of nano materials, in particular to a metal nanowire impact welding device and method based on a laser thermal coupling effect.
Background
With the rapid development of science and technology, compared with the traditional electronics, flexible electronic devices with high flexibility and high deformation rate, such as touch screens, solar cells, light emitting diodes and the like, gradually enter the gate of the electronic field. Flexible electronics is a new electronic technology for fabricating electronic devices of organic and inorganic materials on flexible and ductile substrates. The novel flexible electronic devices should have excellent optoelectronic properties, high transparency, high conductivity and good stability. The transparent conductive electrode is a core structural member of the flexible electronic device, and the preparation material of the transparent conductive electrode is reasonably selected, so that the transparent conductive electrode has very important engineering significance for fully playing the functional characteristics of the flexible electronic device. Indium tin oxide is gradually eliminated as a conventional industrial transparent conductive material due to its many disadvantages such as lack of material resources, high brittleness of material, and high preparation cost. Among a plurality of candidate materials for preparing the transparent conductive electrode (such as carbon nano tube, graphene, conductive polymer, metal grid and metal nano wire), the metal nano wire is the preferred material of the next generation transparent conductive film because of excellent conductivity, flexibility and low preparation cost.
The conducting mechanism of the metal nanowire transparent conducting film is that metal nanowires are arranged in a disordered mode to form a conducting network. The virtual lapping phenomenon among the spatially staggered metal nanowires is a direct reason and a main reason for the fact that the prepared transparent conductive film has large surface resistance and poor deformability, so that the key process for preparing the high-reliability metal nanowire transparent conductive electrode lies in effective welding of metal nanowire contact nodes. The main technical bottleneck restricting the further application of the metal nanowires in the field of flexible electronics at the present stage is how to further improve the welding efficiency and the welding quality of the spatially staggered metal nanowires. The traditional welding method of metal nanowires by high-temperature heating, mechanical pressing and introduction of external media can reduce the node resistance of the metal nanowires to a certain extent, but due to the difference of thermophysical performance parameters between the metal nanowires and the flexible substrate material, great problems still exist in the composite preparation process and the batch engineering application of the flexible transparent conductive film, and the method is specifically represented by the following steps: the upper limit of the heat-resistant temperature of the PET substrate material of the conventional flexible film is low, and the PET substrate material cannot bear the actual high-temperature operation of the metal nanowires at 200 ℃; the welding operation process of the metal nanowires is realized by mechanical pressure, under the action of extremely high pressure stress (often up to 81 GPa), the metal nanowires have the defects of warping, slipping, peeling and the like, and are not suitable for large, fragile and soft substrate materials, in addition, high requirements are required on industrial coating equipment, and the integrated welding cost of the metal nanowires is high; the method for preparing the conductive film by introducing external media (such as PEDOT: PSS, HAuCl4 and the like) has the disadvantages of complex film coating step, low film transmittance, large fog and the like, and can damage the protective layer at the periphery of the nanowire. Therefore, how to provide a novel metal nanowire welding method to achieve high weldability of metal nanowires is one of the problems to be solved urgently at the present stage.
The laser processing has many advantages and characteristics of cleanness, environmental protection, high power density, good controllability, high processing efficiency and the like, and is considered to be one of the methods with great potential for welding the metal nanowire. Currently, scholars in the related field have performed a series of research works, such as: chinese patent publication No. CN112828470A proposes a device and method for laser butt welding of transparent glass, in which two pulsed lasers are emitted by means of a laser generator, and a plasma generated by irradiation of a laser heat source on glass can shield subsequent lasers, so that a plasma region moves from a laser focal region to the laser light source, and fusion welding between glasses is realized. However, the heating method of the patent adopts continuous laser beams to carry out nonlinear heating, the heating object is the whole material to be welded, and the welding quality, the energy utilization efficiency and the welding efficiency have a space for further improving. Chinese patent publication No. CN105149781A proposes a single-point nano welding method based on photothermal effect, in which a continuous laser is used to output monochromatic laser and irradiate to a metal nanowire, and due to the surface plasmon property, photothermal effect is generated, thereby realizing fusion welding operation of the metal nanowire, but due to the complexity of the spatial stacking manner of the metal nanowire, virtual overlap between the metal nanowires may exist, and during actual welding operation, an operation area with poor welding quality may exist, and welding reliability needs to be further improved.
In conclusion, no efficient and high-quality laser welding method for the metal nanowires exists at present. The demand is high, and a novel laser welding method with simple welding process, low welding cost, high controllability, high welding efficiency and excellent welding quality is needed to be provided.
Disclosure of Invention
The invention aims to overcome the defect of poor welding quality caused by virtual overlapping between spatially staggered metal nanowires, and provides a metal nanowire impact welding device and method based on a laser thermal coupling effect, which can improve the welding quality and the welding efficiency of the metal nanowires while realizing the weldability of the metal nanowires.
In order to achieve the purpose, the invention provides the following scheme:
a metal nanowire impact welding device based on a laser thermal coupling effect comprises a laser, a metal nanowire and an online monitoring system;
the laser emits forward laser beams to carry out forward indirect impact operation on the metal nanowires;
meanwhile, the laser emits reverse laser beams to carry out reverse direct heating operation on the metal nanowires;
the upper part of the metal nanowire is sequentially provided with a restraint layer, an absorption layer and a protection layer from top to bottom, and the lower part of the metal nanowire is provided with the restraint layer;
the online monitoring system is used for monitoring the change of the welding behavior of the metal nanowires in real time.
Further, the forward laser beam directly irradiates the absorption layer to generate plasma shock waves, indirectly acts on the metal nanowires through the protective layer, and punches the metal nanowires under the constraint action of the constraint layers on the two sides of the metal nanowires to shorten the distance between the adjacent nanowires; and the reverse laser beam irradiates the metal nanowires to realize effective heating of the adjacent metal nanowire node areas, wherein the node areas are areas with the nanowire lap joint center as the circle center and the diameter range of less than 1 micrometer.
Further, the forward laser beam is a pulse laser, and the backward laser beam can be either a continuous laser or a pulse laser.
Furthermore, the two forward and reverse laser beams can be generated by two lasers respectively, and can also be generated by one laser; the method for generating the two laser beams of the front laser beam and the back laser beam by using one laser comprises the following steps: the single laser is divided into two laser beams by any three or more than three light path management elements of a beam expander, a spectroscope, a reflector or a focusing mirror.
Further, the restraint layer above the metal nanowire is any one of transparent ceramic, BK-7 glass or quartz glass; the restraint layer below the metal nanowire is any one of transparent ceramic, BK-7 glass, quartz glass or a flexible transparent substrate; the absorption layer is any one of graphite, black paint, black adhesive tape or light absorption metal films; the protective layer is any one of pure metals or alloy materials thereof with yield strength lower than 500 MPa.
Further, the online monitoring system comprises a spectrometer and a high-speed camera; the spectrometer is used for observing a dark field scattering spectrum in the metal nanowire welding process in real time, and the high-speed camera is used for observing the shape change in the metal nanowire dynamic welding process in real time; the online monitoring system is used for feeding back the welding condition of the metal nanowire in real time, so as to adjust the process parameters of the laser in real time and realize the closed-loop feedback of the metal nanowire impact welding process; (ii) a The technological parameters of the laser include laser power density, laser frequency, laser wavelength, laser pulse width, laser scanning path, laser scanning speed and the working distance between the laser source and the metal nanometer line.
The invention also provides a metal nanowire impact welding method based on the laser thermal coupling effect, which is characterized by comprising the following steps of:
s1, coating metal nanowires on the surface of a constraint layer;
s2, paving a protective layer material with a surface preset absorption layer above the metal nanowire;
s3, laying another restraint layer above the absorption layer;
and S4, starting a laser, emitting a forward laser beam and a backward laser beam, and completing the welding operation of the metal nanowire by matching with a three-coordinate mobile platform.
Further, in the step S4, the time from the forward laser irradiation to the absorption layer and the time from the reverse laser irradiation to the metal nanowire can be regulated and controlled in a time delay manner, so as to control the sequence and time duration of the laser thermal regulation and control; the intensity of the laser beam can be regulated and controlled by means of the laser energy attenuation device.
Further, in the step S4, the step-by-step laser shock welding of the metal nanowire in the target area can be realized by adopting a single-point stepping manner according to the fixed track; the size and the number of laser spots can be adjusted by beam shaping or adopting any mode of a spatial light modulator, so that single batch laser shock welding of the metal nanowires in the target area is realized.
Furthermore, the centers of the light spots of the forward laser beam and the reverse laser beam coincide, so that the light beam interaction area has an obvious thermal coupling effect.
Compared with the prior art, the invention has the beneficial effects that:
1. compared with an overall nonlinear heating mode of a bulk material, the method has the advantages that local heating of the node region of the staggered metal nanowires is performed by means of the laser plasmon effect, the heating efficiency is higher, and the heating effect is more obvious;
2. the pulse laser is used for impact operation, so that the space between spatially staggered nanowires can be shortened, the phenomenon of virtual lapping is reduced, and the heating effect is enhanced;
3. the original comprehensive mechanical properties of the metal nanowires can be retained to the maximum extent under the condition that the metal nanowires are not melted integrally, and high-reliability welding operation of the spatially staggered nanowires is realized;
4. by means of the online monitoring equipment, the dynamic welding behavior of the metal nanowires can be monitored in real time, welding process parameters are optimized in real time, and then closed-loop feedback of the metal nanowire impact welding process is achieved.
Drawings
Fig. 1 is a schematic diagram of a metal nanowire impact welding method based on a laser thermal coupling effect.
Fig. 2 is a schematic diagram of the position change of the metal nanowire in the impact welding process.
FIG. 3 shows SEM appearances of metal nanowires before and after laser shock assisted welding.
In FIG. 1: 1-forward laser beam; 2-a reverse laser beam; 3-a constraining layer; 4-an absorbing layer; 5-a protective layer; 6-metal nanowires; 7-a spectrometer; 8-high speed camera.
Detailed Description
The technical solution and the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings.
For a better understanding of the present invention, the present invention is further illustrated below with reference to specific examples, which are provided for the purpose of illustration only and are not intended to limit the scope of the present invention.
A metal nanowire impact welding device based on a laser thermal coupling effect comprises a laser, a metal nanowire 6 and an online monitoring system; emitting a forward laser beam 1 by a laser to perform forward indirect impact operation on the metal nanowire, and emitting a reverse laser beam 2 to perform reverse direct heating operation on the metal nanowire; the upper part of the metal nanowire is sequentially provided with a restraint layer 3, an absorption layer 4 and a protective layer 5 from top to bottom, and the lower part of the metal nanowire 6 is provided with the restraint layer 3; the online monitoring system is used for monitoring the welding behavior change of the metal nanowires in real time. The forward laser beam 1 directly irradiates the absorption layer to generate plasma shock waves, indirectly acts on the metal nanowires through the protective layer, and punches the metal nanowires under the constraint of the constraint layers on the two sides of the metal nanowires to shorten the distance between the adjacent metal nanowires; the metal nanowires are irradiated by the reverse laser beam 2, so that the effective heating of the adjacent metal nanowire node areas is realized, and the node areas are areas with the diameter range smaller than 1 micron by taking the nanowire lap joint point center as the circle center. The forward laser beam 1 is a pulsed laser, and the backward laser beam 2 can be either a continuous laser or a pulsed laser. The positive and negative two beams of laser can be generated by two lasers respectively or one laser; the method for generating two laser beams of positive and negative by one laser comprises the following steps: the single laser is divided into two laser beams by any three or more than three light path management elements of a beam expander, a spectroscope, a reflector or a focusing mirror. The restraint layer 3 above the metal nanowire 6 is preferably any one of transparent ceramic, BK-7 glass or quartz glass; the restraint layer 3 below the metal nanowire 6 is any one of transparent ceramic, BK-7 glass, quartz glass or a flexible transparent substrate; the absorption layer 4 is any one of graphite, black paint, black adhesive tape or light absorption metal film; the protective layer 5 is any of pure metals or alloy materials thereof with yield strength lower than 500 MPa. The online monitoring system comprises a spectrometer 7 and a high-speed camera 8; the spectrometer 7 is used for observing dark field scattering spectrum in the welding process of the metal nanowire 6 in real time, and the high-speed camera 8 is used for observing the shape change in the dynamic welding process of the metal nanowire 6 in real time; the online monitoring system is used for feeding back the welding condition of the metal nanowire 6 in real time, so as to adjust the process parameters of the laser in real time and realize the closed-loop feedback of the metal nanowire 6 impact welding process; the technological parameters of the laser include laser power density, laser frequency, laser wavelength, laser pulse width, laser scanning path, laser scanning speed and the working distance between the laser source and the metal nanometer line. The time from the irradiation of the forward laser 1 to the absorption layer and the time from the irradiation of the reverse laser 2 to the metal nanowire 6 can be regulated and controlled in a time delay mode, so that the sequence and the time length of the laser thermal regulation are controlled; the intensity of the laser beam can be regulated and controlled by means of the laser energy attenuation device. The gradual laser shock welding of the metal nanowire 6 in the target area can be realized by adopting a single-point stepping mode according to the fixed track; the size and the number of the laser spots can be adjusted by beam shaping or a spatial light modulator, so that single batch laser impact welding of the metal nanowires in the target area is realized. The centers of the light spots of the forward laser beam and the reverse laser beam are overlapped, so that the light beam interaction area has an obvious thermal coupling effect.
The specific embodiment is as follows:
example 1: laser welding of spatially interleaved copper metal nanowires
Fig. 1 shows a metal nanowire impact welding method based on the laser thermal coupling effect in this embodiment. The specific implementation steps are as follows:
s1: cleaning quartz glass (thickness is 1 mm) of the material of the constraint layer by using an acetone solvent and an ultrasonic cleaning machine;
s2: coating copper metal nanowires on the surface of the cleaned quartz glass;
s3: laying an aluminum foil (the thickness is 5 mu m) with a graphite layer preset on the surface above the copper metal nanowire;
s4: paving another quartz glass (the thickness is 1 mm) on the surface of the preset graphite layer, and further shortening the spacing between the constraint layer, the absorption layer and the protective layer by adopting a locking device;
s5: a nanosecond pulse laser (laser wavelength of 1064nm, pulse width of 7ns, pulse frequency of 1Hz, current of 10A, voltage of 670V, and laser single pulse energy of) is selected. The nanosecond pulse laser is started, a pulse laser beam is emitted, the pulse laser is divided into pulse laser beams with the wavelengths of 1064nm and 532nm by means of an interference cut-off filter, wherein the laser with the wavelength of 1064nm is reflected by a reflecting mirror, then is focused by a focusing mirror, penetrates through quartz glass and directly acts on the surface of the graphite layer, and the other laser with the wavelength of 532nm is reflected by the reflecting mirror and then is focused on the surface of the metal nanowire by the focusing mirror. And (3) matching with a three-coordinate moving platform (the moving speed is 0.1 mm/S), and adopting an S-shaped scanning path to complete the welding operation of the spatially staggered copper metal nanowires in the target area.
Fig. 2 is a schematic diagram showing the position change of the metal nanowire in the present impact welding process. The welding operation mechanism of the copper metal nanowire in the embodiment is as follows: the method has the advantages that local heating of the node area of the staggered metal nanowires is carried out by means of a reverse laser plasmon effect, impact operation is carried out by means of forward pulse laser, the distance between adjacent nanowires is shortened, the virtual lapping phenomenon is reduced, the heating effect is enhanced, the original comprehensive mechanical property of the metal nanowires is retained to the maximum extent under the condition that the metal nanowires are not melted integrally, and high-reliability welding operation of the spatially staggered nanowires is achieved.
As shown in fig. 3, the SEM morphology of the copper metal nanowires before and after the laser shock assisted welding in this embodiment is shown. Observing the partial graph (a), when the impact operation is not carried out by adopting the forward pulse laser, namely when the irradiation operation is carried out by only adopting the reverse heating laser, the welding quality of the metal nanowire is poor, and the melting appearance appears only at the end position of the nanowire. Comparing the partial graph (a) and observing the partial graph (b), the result shows that when the forward pulse laser is compounded, the forward laser and the reverse laser are simultaneously adopted for processing, and the large-area welding of the spatially staggered nanowires is realized.
Example 2: laser welding of spatially interleaved copper metal nanowires on polyethylene terephthalate (PET) substrate surface
Fig. 1 shows a metal nanowire impact welding method based on the laser thermal coupling effect in this embodiment. The specific implementation steps are as follows:
s1: the PET substrate material was cleaned with ethanol and distilled water for 10min with the help of an ultrasonic cleaner.
S2: and uniformly coating the copper metal nanowires on the surface of the PET substrate by adopting a bar coater.
S3: laying an aluminum foil (the thickness is 5 mu m) with a graphite layer preset on the surface above the copper metal nanowire;
s4: rolling the PET substrate, the copper metal nanowires and the aluminum foil with a preset graphite layer in real time by using a BK-7 cylindrical roller;
s5: a nanosecond pulse laser (laser wavelength of 1064nm, pulse width of 7ns, pulse frequency of 1Hz, current of 10A, voltage of 670V, and laser single pulse energy of 345 mJ) is selected. The nanosecond pulse laser is started, a pulse laser beam is emitted, the pulse laser is divided into pulse laser beams with the wavelengths of 1064nm and 532nm by means of an interference cut-off filter, wherein the laser with the wavelength of 1064nm is reflected by a reflecting mirror, then is focused by a focusing mirror, penetrates through quartz glass and directly acts on the surface of the graphite layer, and the other laser with the wavelength of 532nm is reflected by the reflecting mirror and then is focused on the surface of the metal nanowire by the focusing mirror. And (3) matching with a three-coordinate moving platform (the moving speed is 0.1 mm/S), and adopting an S-shaped scanning path to complete the welding operation of the spatially staggered copper metal nanowires in the target area.
Fig. 2 is a schematic diagram showing the position change of the metal nanowires in the impact welding process. In this example, laser welding of copper metal nanowires was spatially staggered on the surface of polyethylene terephthalate (PET) substrate: the method has the advantages that local heating of the node area of the interlaced metal nanowires is carried out by means of the reverse laser plasmon effect, impact operation is carried out by means of forward pulse laser, the space interlaced nanowire distance is shortened, the virtual lapping phenomenon is reduced, the heating effect is enhanced, the original comprehensive mechanical property of the metal nanowires is retained to the maximum extent under the condition that the metal nanowires are not melted integrally, and high-reliability welding operation of the space interlaced nanowires is achieved.
Finally, it should be noted that: the above description is only intended to illustrate the technical solution of the present invention, and not to limit it; although the invention has been described in detail with reference to specific embodiments, those skilled in the art will understand that: the technical solutions described in the foregoing embodiments may be modified, or some technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A metal nanowire impact welding device based on a laser thermal coupling effect is characterized by comprising a laser, a metal nanowire and an online monitoring system;
the laser emits forward laser beams to carry out forward indirect impact operation on the metal nanowires;
meanwhile, the laser emits reverse laser beams to carry out reverse direct heating operation on the metal nanowires;
the upper part of the metal nanowire is sequentially provided with a restraint layer, an absorption layer and a protection layer from top to bottom, and the lower part of the metal nanowire is provided with the restraint layer;
the online monitoring system is used for monitoring the welding behavior change of the metal nanowires in real time.
2. The metal nanowire impact welding device based on the laser thermal coupling effect as claimed in claim 1, wherein the forward laser beam generates plasma shock waves by directly irradiating the absorption layer, indirectly acts on the metal nanowires through the protection layer, and punches the metal nanowires under the constraint action of the constraint layers on two sides of the metal nanowires to shorten the distance between the adjacent nanowires; and the reverse laser beam irradiates the metal nanowires to realize effective heating of the adjacent metal nanowire node areas, wherein the node areas are areas with the nanowire lap joint center as the circle center and the diameter range of less than 1 micrometer.
3. The metal nanowire impact welding device based on the laser thermal coupling effect as claimed in claim 1, wherein the forward laser beam is a pulse laser, and the backward laser beam can be either a continuous laser or a pulse laser.
4. The metal nanowire impact welding device based on the laser thermal coupling effect as claimed in claim 1, wherein the two laser beams can be generated by two lasers respectively or one laser; the method for generating the two laser beams of the front laser beam and the back laser beam by using one laser comprises the following steps: the single laser is divided into two laser beams by any three or more than three light path management elements of a beam expander, a spectroscope, a reflector or a focusing mirror.
5. The metal nanowire impact welding device based on the laser thermal coupling effect as claimed in claim 1, wherein the constraining layer above the metal nanowires is any one of transparent ceramic, BK-7 glass or quartz glass; the restraint layer below the metal nanowire is any one of transparent ceramic, BK-7 glass, quartz glass or a flexible transparent substrate; the absorption layer is any one of graphite, black paint, black adhesive tape or light absorption metal films; the protective layer is any one of pure metals or alloy materials thereof with yield strength lower than 500 MPa.
6. The metal nanowire impact welding device based on the laser thermal coupling effect as claimed in claim 1, wherein the on-line monitoring system comprises a spectrometer and a high-speed camera; the spectrometer is used for observing dark field scattering spectrum in the metal nanowire welding process in real time, and the high-speed camera is used for observing morphology change in the metal nanowire dynamic welding process in real time; the online monitoring system is used for feeding back the welding condition of the metal nanowires in real time, so as to adjust the process parameters of the laser in real time and realize the closed-loop feedback of the metal nanowire impact welding process; the technological parameters of the laser include laser power density, laser frequency, laser wavelength, laser pulse width, laser scanning path, laser scanning speed and the working distance between the laser source and the metal nanometer line.
7. The metal nanowire impact welding method based on the laser thermal coupling effect according to any one of claims 1 to 6, characterized by comprising the following steps:
s1, coating metal nanowires on the surface of a constraint layer;
s2, paving a protective layer material with a surface preset absorption layer above the metal nanowire;
s3, laying another restraint layer above the absorption layer;
and S4, starting a laser, emitting positive and negative laser beams, and completing the welding operation of the metal nanowire by matching with a three-coordinate mobile platform.
8. The metal nanowire impact welding method based on the laser thermal coupling effect according to claim 7, wherein in the step S4, the time from the forward laser irradiation to the absorption layer and the time from the reverse laser irradiation to the metal nanowire can be adjusted and controlled in a time delay manner, so as to control the sequence and the time length of the laser thermal adjustment; the intensity of the laser beam can be regulated and controlled by means of the laser energy attenuation device.
9. The metal nanowire impact welding method based on the laser thermal coupling effect as claimed in claim 7, wherein in step S4, the step-by-step laser impact welding of the metal nanowire in the target area can be realized by adopting a single-point stepping manner according to a fixed track; the size and the number of laser spots can be adjusted by beam shaping or adopting any mode of a spatial light modulator, so that single batch laser shock welding of the metal nanowires in the target area is realized.
10. The metal nanowire impact welding method based on the laser thermal coupling effect as claimed in claim 7, wherein the centers of the light spots of the forward laser beam and the backward laser beam coincide to realize that the beam interaction region has the obvious thermal coupling effect.
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