CN111549339B - Method for enhancing bonding fastness of graphene and base material - Google Patents
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Abstract
The invention discloses a method for enhancing the bonding fastness of graphene and a base material, which comprises the following steps: s1, preparing a combined sample by liquid-phase coating or cladding of graphene on the surface of a base material; s2, mounting the sample prepared in the S1 on an electric three-dimensional movable platform in a vacuum chamber for later use; s3, opening the laser, and focusing the light path of the laser on the sample in the S2; s4, burning the laser by focusing on a planned point of a sample to quickly form plasma, introducing functional groups, and grafting and combining by utilizing electrons and particles, and relates to the technical field of graphene. According to the method for enhancing the bonding fastness of the graphene and the base material, the plasma is rapidly formed by directly adopting a laser ablation method, functional groups are introduced, and the bonding fastness of different base materials cladded by the graphene is enhanced by utilizing electron and ion grafting and bonding. The graphene and the base material can obtain a bound structure with higher bonding strength through the change of an external electromagnetic field, so that the bonding of two materials with more stable surfaces is realized.
Description
Technical Field
The invention relates to the technical field of graphene, in particular to a method for enhancing the bonding fastness of graphene and a base material.
Background
Graphene has excellent physical properties, and each excellent physical property lays a foundation for the development of the graphene in the application field, but the ultra-thin two-dimensional structure of the graphene determines that the graphene is difficult to be used independently, and the properties can be expressed only by depending on a certain substrate to form a graphene composite material, at present, the preparation methods of the graphene composite material mainly comprise two methods: one method comprises the steps of coating a graphene film on the surface of a base material by a liquid-phase coating method by using liquid-phase exfoliated graphene or reduced graphene oxide as a raw material; the other is that graphene growing on the surface of a metal substrate by a chemical vapor deposition method is used as a raw material, a graphene film is transferred to the surface of a substrate by a transfer method, and in a liquid-phase coating method, due to the small size, many defects and uneven layer number of graphene sheets, the uniformity of the graphene film obtained by spin coating is poor and has a large difference from the theoretical performance, and the film and the substrate do not have the effect of chemical bonds, so that the bonding fastness is low.
However, in the process of transferring graphene growing on the surface of a metal substrate to the surface of another substrate, due to the use of a liquid phase chemical reagent, the problem of graphene pollution is caused, the transfer process is complicated, defects, wrinkles and the like of graphene are easily caused, and these factors greatly restrict the performance of the obtained graphene.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for enhancing the bonding fastness of graphene and a base material, and solves the problem of low bonding fastness between a film and a substrate in common methods such as liquid-phase coating and the like.
In order to achieve the purpose, the invention is realized by the following technical scheme: a method for enhancing the bonding fastness of graphene and a substrate comprises the following steps:
s1, preparing a combined sample by coating or cladding a graphene liquid phase on the surface of a base material;
s2, mounting the sample prepared in the S1 on an electric three-dimensional movable platform in a vacuum chamber for later use;
s3, opening the laser, and focusing the light path of the laser on the sample in the S2;
s4, laser is focused on a planned point of a sample to be burnt, plasma is quickly formed, functional groups are introduced, and the bonding strength of graphene coated on the base material is enhanced by utilizing electron and particle grafting and bonding.
Further, the substrate in S1 includes glass, silicone rubber, ceramic, lorentz and metal, and graphene is directly coated on the surface of the substrate by a coating method when a sample is prepared, so that the graphene forms a thin film. Effectively prevents the sample from being damaged due to air oxidation in laser ablation
Further, the sample in the step S2 is fixed with an electric three-dimensional movable platform, the electric three-dimensional movable platform is positioned in the vacuum chamber, and the vacuum chamber is in a sealed state when the vacuum chamber is used.
Further, the electric three-dimensional movable platform can be adjusted according to the requirement of an ablation point of the sample, so that the moving position and speed of the sample can be controlled.
Further, when the laser in the S4 is focused on the surface of a product in the vacuum chamber, an emission spectrum and a Raman spectrum are generated, the emission spectrum and the Raman spectrum are transmitted to a spectrometer through a receiver and an optical fiber for light splitting, and the spectrum is taken through an ICCD and a spectrum signal is converted into an electric signal to be transmitted to a computer.
Furthermore, a pulse digital delayer is arranged at the input end of the laser, and the triggering delay of the laser and the ICCD can be adjusted.
Furthermore, a scanning tunnel microscope is arranged on one side of the vacuum chamber, and the output end of the scanning tunnel microscope is matched with the vacuum chamber, so that the interface can be observed in real time and the graphene can be represented.
A microscope position adjustment platform for adjusting and fixing a scanning tunneling microscope in the method for enhancing the bonding fastness of graphene and a substrate, the microscope position adjustment platform comprising:
the fixed case, the bottom fixedly connected with lift motor of the inner wall of fixed case, lift motor's output fixedly connected with lift screw, lift screw's surperficial threaded connection has the linkage board, two at least lift axles of top fixedly connected with of linkage board, at least two the top fixedly connected with backup pad of lift axle, the sliding tray has been seted up at the top of backup pad, two fixed axles of inside fixedly connected with of backup pad, two the equal sliding connection in surface of fixed axle has the removal slider, two the top fixedly connected with mounting panel of removal slider, the bottom fixedly connected with movable plate of mounting panel, the inside fixedly connected with of sliding tray removes the telescopic link, the output of removing the telescopic link with one side fixed connection of movable plate, the bottom fixedly connected with height detection chi of backup pad.
Furthermore, the top ends of at least two lifting shafts penetrate through the fixed box and extend to the upper side of the fixed box, the at least two lifting shafts are vertically distributed with the surface of the linkage plate, and the at least two lifting shafts are parallel to each other.
Furthermore, the two fixing shafts are parallel to each other, and the bottom end of the height detection ruler penetrates through the fixing box and extends to the inside of the fixing box.
Compared with the prior art, the invention has the beneficial effects that:
according to the method for enhancing the bonding fastness of the graphene and the base material, the plasma is rapidly formed by directly adopting a laser ablation method, functional groups are introduced, and the bonding fastness of different base materials cladded by the graphene is enhanced by utilizing electron and ion grafting and bonding. The graphene and the base material can obtain a bound structure with higher bonding strength through the change of an external electromagnetic field, so that the bonding of two materials with more stable surfaces is realized.
Drawings
Fig. 1 is a system diagram of a method for enhancing the bonding fastness of graphene and a substrate according to the present invention;
FIG. 2 is a schematic structural diagram of a microscope position adjustment stage according to the present invention;
fig. 3 is a schematic structural view of the support plate portion shown in fig. 2 according to the present invention.
In the figure: 1-laser, 2-vacuum chamber, 3-minced noodle tunneling microscope, 4-receiver, 5-spectrometer, 6-ICCD, 7-computer, 8-pulse digital delayer, 9-fixed box, 91-lifting motor, 92-lifting screw, 93-linkage plate, 94-lifting shaft, 95-support plate, 951-sliding groove, 96-fixed shaft, 97-movable sliding block, 98-mounting plate, 981-movable plate, 99-movable telescopic rod and 10-height detection ruler.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Referring to fig. 1-3, the present invention provides a technical solution: a method for enhancing the bonding fastness of graphene and a substrate comprises the following steps:
s1, preparing a combined sample by coating or cladding a graphene liquid phase on the surface of a base material;
s2, mounting the sample prepared in the S1 on an electric three-dimensional movable platform in a vacuum chamber 2 for later use;
s3, opening the laser 1, and focusing the light path of the laser 1 on the sample in the S2;
s4, the laser 1 is focused on a planned point of a sample to be burned, plasma is quickly formed, functional groups are introduced, and the bonding strength of graphene fused on the base material is enhanced by utilizing electron and particle grafting and bonding.
The planning point is determined by setting the moving mode of the mobile platform through software.
The method directly adopts a laser ablation method to quickly form plasma, introduces functional groups, and utilizes electron and ion grafting and combination to enhance the combination fastness of different substrates cladded by graphene. The graphene and the base material can obtain a bound structure with higher bonding strength through the change of an external electromagnetic field, so that the bonding of two materials with more stable surfaces is realized.
The laser 1 has the characteristics of monochromaticity, high directionality, concentrated energy distribution and the like, is widely applied in the field of material processing, commercialization of ultraviolet, infrared, visible light and tunable lasers and simplification of structures thereof, greatly expands the selection range of laser processing methods, reduces the cost of laser processing methods, improves the efficiency, and enables the materials to show high application value in the field of material processing, band gap-free graphene hinders the wide application of the magic materials, artificial dynamic band gaps can be manufactured by irradiating graphene with laser, along with the development of laser technology and electronic science technology, the research on the physical chemistry and mechanical property stability of graphene materials under the action of laser is very important for the development and development of optoelectronic devices and the like, meanwhile, the research on the defect characteristics of graphene materials under the action of laser plays a decisive role in understanding and predicting certain characteristics of graphene materials, experiments prove that the carbon materials can be mutually transformed by irradiating the carbon materials with laser, the laser can be transformed into carbon plasmas, the planar deposition of carbon atoms can be realized by changing the surrounding environment when the carbon plasmas are cooled during the laser action, so that the planar deposition of the graphene can be mutually transformed with different phase structures, the graphene can be manufactured by utilizing the mutual transformation of the conventional graphene, the functions of graphene, the graphene can be effectively reduced and the graphene, and the graphene can be manufactured by utilizing the in-situ laser technology of the conventional graphene, and the in-situ laser, the in-process of the graphene, and the graphene, the graphene can be effectively reducing and the graphene.
The laser burns only a very small local area of the surface of the candle sample, and the mass of the candle-stripping sample is as small as tens to hundreds of nanograms, which is also often regarded as a non-destructive ablation means.
The substrate in the S1 comprises glass, silicon rubber, ceramic, lorentz and metal, and graphene is directly coated on the surface of the substrate through a coating method during sample preparation, so that the graphene forms a film.
Different materials such as glass, silicon rubber, ceramic, lorentz and metal are used as base materials, graphene covers the surface of the base materials to form a layer of film, the two materials are combined through a common film coating method, in order to prevent air oxidation during laser ablation and increase sample damage, a sample is placed in a vacuum chamber and is fixed on an electric three-dimensional movable platform.
Effectively prevents the sample from being damaged due to air oxidation in laser ablation.
And in the S2, the sample and the electric three-dimensional movable platform are fixed, the electric three-dimensional movable platform is positioned in the vacuum chamber 2, and the vacuum chamber 2 is in a sealed state during use.
Plasma is generated through pulsed laser ablation, so that different substrates such as graphene cladding glass, silicon rubber, ceramic, lorentz and metal materials are made; the experimental parameters such as laser power, laser pulse frequency, lens focal length, laser ablation time, acquisition orientation, acquisition delay and the like need to be optimized for different base materials.
The electric three-dimensional movable platform can be adjusted according to the requirement of an ablation point of the sample, so that the moving position and the moving speed of the sample are controlled.
In the S4, when the laser 1 is focused on the surface of a product in the vacuum chamber 2, an emission spectrum and a Raman spectrum are generated, the emission spectrum and the Raman spectrum are transmitted to a spectrometer 5 through a receiver 4 and an optical fiber for light splitting, the spectrum is captured through an ICCD6, and a spectrum signal is converted into an electric signal to be transmitted to a computer 7.
The input end of the laser 1 is provided with a pulse digital delayer 8 which can adjust the triggering delay of the laser and the ICCD.
One side of the vacuum chamber 2 is provided with a scanning tunnel microscope 3, and the output end of the scanning tunnel microscope 3 is matched with the vacuum chamber 2, so that the interface can be observed in real time and the graphene can be represented.
Focusing laser 1 on the surface of a sample to generate an emission spectrum and a Raman spectrum, transmitting the emission spectrum and the Raman spectrum to a spectrometer 5 through a receiver 4 and an optical fiber for light splitting, carrying out ICCD6 spectrum shooting, converting spectrum information into telecommunication signals and transmitting the telecommunication signals to a computer, changing the changes of laser parameters, sample temperature, current and the like, analyzing the spectrum information by collecting the plasma emission spectrum on the surface of the material before and after ablation, and analyzing the performance change of the material before and after ablation by combining the evolution characteristic of the plasma; and (4) observing the influence of the laser ablation on the graphene substrate structure by combining Raman spectrum characterization and a tunneling microscope.
And for the spectrum results obtained by researching the binding fastness and the performance stability of the material through laser ablation, the related binding fastness and performance stability results are obtained by comparing the difference of the two acquisition results.
When the graphene cladding material is in work, plasma is directly and rapidly formed by a laser ablation method, functional groups are introduced, the bonding fastness of different graphene cladding base materials is enhanced by utilizing electron and ion grafting and bonding, a binding structure with higher bonding strength can be obtained by the graphene and the base materials through the change of an external electromagnetic field, and therefore the bonding of two materials with more stable surfaces is realized.
A microscope position adjustment stage for adjusting and fixing a scanning tunnel microscope 3, the microscope position adjustment stage comprising:
During actual use, the scanning tunnel microscope 3 is fixedly arranged above the mounting plate 98, the movable plate 981 is driven to synchronously move by the movable telescopic rod 99, the movable plate 981 synchronously drives the mounting plate 98 to move, and the mounting plate 98 synchronously drives the scanning tunnel microscope 3 to move, so that the horizontal distance of the scanning tunnel microscope 3 can be conveniently adjusted, the scanning tunnel microscope 3 does not need to be lifted or pushed to move independently, the stability during moving is ensured, and the increase of adjusting time caused by the change of the angle and the observation position of the scanning tunnel microscope 3 due to the fact that the scanning tunnel microscope 3 is touched by mistake is avoided;
the lifting motor 91 at the bottom drives the lifting screw 92 to synchronously rotate, the lifting screw 92 synchronously drives the linkage plate 93 to move up and down for adjustment through a threaded connection structure, the two lifting shafts 94 at the top synchronously drive the supporting plate 95 to move up and down for adjustment when the linkage plate 93 moves up and down, the supporting plate 95 synchronously drives the mounting plate 98 at the top to move up, and the mounting plate 98 synchronously drives the scanning tunnel microscope 3 above to carry out height adjustment so as to adapt to the use requirements of the scanning tunnel microscope 3 on different heights and conveniently adjust the position of the scanning tunnel microscope;
the backup pad 95 drives the height detection chi 10 in step and reciprocates when reciprocating the regulation and reciprocates, and when the bottom of backup pad 95 and the top contact of fixed case 9, the top of fixed case 9 corresponds the zero scale department of height detection chi 10, and when the backup pad 95 upwards moved gradually, the scale that height detection chi 10 and fixed case 9's top correspond increased gradually to the distance that risees to backup pad 95 carries out quick accurate measuring.
The top ends of at least two lifting shafts 94 penetrate through the fixed box 9 and extend to the upper part of the fixed box 9, the at least two lifting shafts 94 are vertically distributed with the surface of the linkage plate 93, and the at least two lifting shafts 94 are parallel to each other.
The two fixing shafts 96 are parallel to each other, and the bottom end of the height detection ruler 10 penetrates through the fixing box 9 and extends into the fixing box 9.
When the lifting motor 91 is used, an external power supply and a control switch are connected, and the starting and stopping of the lifting motor 91 are controlled through the control switch.
When in use:
the movable rod 99 is moved to drive the movable plate 981 to move synchronously, the movable plate 981 is moved to drive the mounting plate 98 to move synchronously, and the mounting plate 98 is moved synchronously to drive the scanning tunnel microscope 3 to move, so that the horizontal distance of the scanning tunnel microscope 3 can be adjusted conveniently, the scanning tunnel microscope 3 does not need to be lifted or pushed independently to move, the stability during moving is guaranteed, and the phenomenon that the angle and the observation position of the scanning tunnel microscope 3 are changed to increase the adjusting time due to mistaken touch of the scanning tunnel microscope 3 is avoided;
the lifting motor 91 at the bottom drives the lifting screw 92 to synchronously rotate, the lifting screw 92 synchronously drives the linkage plate 93 to move up and down for adjustment through a threaded connection structure, the two lifting shafts 94 at the top synchronously drive the supporting plate 95 to move up and down for adjustment when the linkage plate 93 moves up and down, the supporting plate 95 synchronously drives the mounting plate 98 at the top to move up, and the mounting plate 98 synchronously drives the scanning tunnel microscope 3 above to carry out height adjustment so as to adapt to the use requirements of the scanning tunnel microscope 3 on different heights and conveniently adjust the position of the scanning tunnel microscope;
the backup pad 95 drives the height detection chi 10 in step and reciprocates when reciprocating the regulation and reciprocates, and when the bottom of backup pad 95 and the top contact of fixed case 9, the top of fixed case 9 corresponds the zero scale department of height detection chi 10, and when the backup pad 95 upwards moved gradually, the scale that height detection chi 10 and fixed case 9's top correspond increased gradually to the distance that risees to backup pad 95 carries out quick accurate measuring.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (3)
1. A method for enhancing the bonding fastness of graphene and a substrate is characterized by comprising the following steps:
s1, preparing a combined sample by coating or cladding graphene liquid phase on the surface of a rotating base material;
s2, mounting the sample prepared in the S1 on an electric three-dimensional movable platform in a vacuum chamber for later use;
s3, opening the laser, and focusing the light path of the laser on the sample in the S2;
s4, firing the laser by focusing on a planned point of the sample to quickly form plasma, introducing functional groups, and enhancing the bonding strength of the graphene coated on the base material by utilizing electron and particle grafting and bonding;
the substrate in the S1 comprises glass, silicon rubber, ceramic, loran and metal, and graphene is directly coated on the surface of the substrate by a coating method during sample preparation, so that the graphene forms a film;
the sample in the S2 is fixed with the electric three-dimensional movable platform, the electric three-dimensional movable platform is positioned in the vacuum chamber, and the vacuum chamber is in a sealed state when in use;
the electric three-dimensional movable platform can be adjusted according to the requirement of an ablation point of a sample, so that the moving position and speed of the sample are controlled;
in S4, when the laser is focused on the surface of a product in the vacuum chamber, an emission spectrum and a Raman spectrum are generated, the emission spectrum and the Raman spectrum are transmitted to a spectrometer through a receiver and an optical fiber for light splitting, and the spectrum is captured through an ICCD (integrated chip CD) and a spectrum signal is converted into an electric signal to be transmitted to a computer;
the input end of the laser is provided with a pulse digital delayer which can adjust the triggering delay of the laser and the ICCD;
a scanning tunnel microscope is arranged on one side of the vacuum chamber, and the output end of the scanning tunnel microscope is matched with the vacuum chamber, so that the interface can be observed in real time and the graphene can be represented;
focusing laser on the surface of a sample to generate an emission spectrum and a Raman spectrum, carrying out light splitting on the emission spectrum and the Raman spectrum through a receiver and an optical fiber to a spectrometer, carrying out ICCD spectrography, converting spectrum information into an electric signal and transmitting the electric signal to a computer, changing laser parameters, sample temperature, current and other changes, analyzing the spectrum information by collecting the plasma emission spectrum on the surface of the material before and after ablation, and analyzing the performance change of the material before and after ablation by combining the evolution characteristic of the plasma; observing the influence of laser ablation on the graphene substrate structure by combining Raman spectrum characterization and a scanning tunnel microscope;
for the spectrum result obtained by researching the binding fastness and the performance stability of the material by laser ablation, the related binding fastness and performance stability results are obtained by comparing the difference of the two acquisition results;
a microscope position adjustment stage for adjusting and fixing the scanning tunneling microscope includes:
the fixed case, the bottom fixedly connected with elevator motor of the inner wall of fixed case, elevator motor's output fixedly connected with lifting screw, lifting screw's surperficial threaded connection has the linkage board, two at least lift axles of top fixedly connected with of linkage board, at least two the top fixedly connected with backup pad of lift axle, the sliding tray has been seted up at the top of backup pad, two fixed axles of the inside fixedly connected with of backup pad, two the equal sliding connection in surface of fixed axle has the removal slider, two the top fixedly connected with mounting panel of removal slider, the bottom fixedly connected with movable plate of mounting panel, the inside fixedly connected with of sliding tray removes the telescopic link, the output of removing the telescopic link with one side fixed connection of movable plate, the bottom fixedly connected with height detection chi of backup pad.
2. The method of claim 1, wherein top ends of at least two of the lifting shafts penetrate through the fixed box and extend above the fixed box, the at least two of the lifting shafts are perpendicular to a surface of the linkage plate, and the at least two of the lifting shafts are parallel to each other.
3. The method for enhancing the bonding fastness of graphene and a substrate according to claim 2, wherein the two fixed shafts are parallel to each other, and the bottom end of the height detection ruler penetrates through the fixed box and extends to the inside of the fixed box.
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| CN101776434B (en) * | 2010-03-10 | 2011-12-14 | 南开大学 | Method and device for measuring small blind hole based on tunnel current feedback collimation |
| CN103508450B (en) * | 2013-09-11 | 2015-05-20 | 清华大学 | Laser preparation method for large-area patterned graphene |
| CN106222650A (en) * | 2016-07-29 | 2016-12-14 | 苏州大学张家港工业技术研究院 | The surface reinforcing method of laser-impact graphite oxide ene coatings |
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