CN113929085B - Three-dimensional patterned porous graphene blackbody and preparation method and application thereof - Google Patents
Three-dimensional patterned porous graphene blackbody and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a method for realizing three-dimensional patterning multistage structure construction of a carbonaceous material by utilizing a short pulse or ultrashort pulse laser direct gasification method, preparing a carbonaceous blackbody material, and applying the carbonaceous blackbody material to the fields of wide-spectrum light absorption, a supercapacitor, nano catalysis and the like, and relates to the technical fields of solar energy or spectral absorption utilization, battery energy, environmental management and the like.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a three-dimensional patterned porous graphene black body prepared by a short pulse laser processing method, a preparation method and application thereof.
Background
Graphene is a two-dimensional layered novel material formed by single-layer carbon atom lattice arrangement, is a novel material integrating excellent electrical conductivity, high mobility, high thermal conductivity, high specific surface area and excellent mechanical properties, and particularly has wide application prospects in various fields of photoelectrons, composite materials, energy storage, energy capture, thermal management, catalysis and the like.
Hitherto, various methods for preparing graphene have been developed such as a mechanical exfoliation method, an ultrasonic exfoliation method, a chemical synthesis method, a chemical vapor deposition method, a graphite oxide reduction method, etc., but these methods can only prepare graphene having a small size, and cannot obtain a porous graphene material having a three-dimensional structure in a large area. The yield of graphene single-layer and few-layer graphene prepared by the ultrasonic stripping method is low, the utilization rate of raw materials is low, and the prepared graphene is easy to agglomerate. The graphene material prepared by the chemical vapor deposition method needs to use copper foil, foam nickel and other catalysts and a bottom material, needs high temperature, has higher equipment and process cost, and needs a complex transfer process to obtain the pure graphene material. Graphene prepared by a graphite oxide reduction method contains a large number of chemical defects, and the microstructure of the graphene only has a two-dimensional lamellar shape, but not a three-dimensional porous structure, so that a blackbody structure with a three-dimensional porous micro-nano structure cannot be formed. Meanwhile, the graphene prepared by the method often requires an additional patterning process to obtain the graphene with a specific pattern structure.
On the other hand, large-scale preparation of graphene often requires high-cost vacuum equipment or consumes chemical reagents for carbon source, transfer, dispersion and deposition, and has the defects of more byproducts, complex process and limitation of high-efficiency and low-cost preparation of graphene. The novel graphene preparation and patterning method with simple development, high efficiency and simple process is used for preparing the three-dimensional porous graphene black body, and has important significance.
In 2012, the Richard b.kaner group, university of california, los angeles, usa, uniformly coated graphite oxide on the surface of an optical disc, and a laser in a DVD optical disc drive was used to heat the reduced graphite oxide to obtain a graphene film (m.el-Kady, r.kaner, nature Communications,4,1475, 2013) with higher conductivity (1738S/m). However, the method is only to heat and reduce the graphene oxide material, the graphene oxide is still required to be used as a raw material, the micro-nano scale patterning of the graphene film cannot be performed, and the graphene black body material with the three-dimensional nano structure cannot be formed.
In 2014, james Tour group of university of rice in united states prepared porous graphene using laser ablation method with commercial polymer film as precursor (J.Lin, Z.Peng, Y.Liu, F.Ruiz-zepeta, R.Ye, E.L.G.Samuel, M.J.Yacaman, B.I.Yakobson, J.M.Tour, nature Communications,5,5714, 2014). The authors use CO 2 The infrared laser is used as a light source, the polyimide film is used as carbon, and the laser-induced graphite is preparedThe graphene is only extended from a graphite material prepared from classical polyimide, the obtained polycrystalline few-layer graphene has no sublimation phenomenon of carbon element under the action of laser, and the graphene has no controllable three-dimensional structure, namely, cannot form a graphene black body.
Patent number: 202010163115.8A method for preparing a porous graphene film by processing a polyimide film by laser is provided, and the high polymer is converted into graphene. However, this patent has the following drawbacks: 1) Polyimide materials are high in price and single in variety; 2) The fine processing of the nano-microstructure of the material by laser is difficult to realize, and a three-dimensional blackbody-like nano-microstructure cannot be formed.
In 2015, the university of Qinghua Zhong Minlin teaches that the subject group adopts femtosecond laser cutting to pattern the graphene grown by a chemical vapor deposition method (Lin, she Xiaohui, han Jinpeng, fan Peixun, zhong Minlin, chinese laser, 2015,42 (7), 0703002), so that the influence of the femtosecond laser energy density and the scanning speed on the cutting of the graphene is studied, and the cutting of different complex patterns of graphene is realized. However, the method still depends on graphene prepared by a chemical vapor deposition method as a raw material, and the femtosecond laser equipment is high in price and the graphene is easy to remain in the femtosecond laser cutting process.
Fresh water resources in the world are in a very severe situation, and according to the predictions of relevant organizations of united nations, fresh water in the 21 st century becomes the most intense natural resource in the world. However, seawater resources are quite abundant, and seawater desalination technology is considered as a long-term effective way to solve the shortage of fresh water resources. Currently, sea water desalination technologies mainly include distillation, electrodialysis, reverse Osmosis (RO) technologies, and the like. The most widely used of these are multistage flash (MSF) and Reverse Osmosis (RO) technologies. Multistage flash evaporation (MSF) mainly faces the problems of high energy consumption and relatively complex structure, and Reverse Osmosis (RO) technology mainly has the conditions of membrane service life, pollution resistance and the like.
In recent years, a technology for realizing interface evaporation by utilizing solar local heat has been developed to a certain extent, and the technology gradually goes from a laboratory to practical application. The technology is environment-friendly and low in energy consumption, and the novel blackbody-like material with a special micro-nano structure is mainly used as a carrier to efficiently utilize sunlight, so that the efficient utilization of heat is realized. At present, the technology mainly depends on the nano material which is relatively expensive and has complex preparation process, so the nano material which is cheap and easy to obtain, has excellent light absorption performance and developed pore structure, and the low-cost and high-efficiency preparation method thereof are a necessary requirement.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing a patterned porous graphene blackbody with a three-dimensional micro-nano structure by using a laser processing method, a preparation method and application thereof. The biomass carbon material, the carbonaceous sponge, the foam, the gel, the film, the activated carbon, the mesoporous carbon and the like are treated by a laser processing method, the carbonaceous material is converted to the graphitization direction by the local photo-thermal effect of laser, the porous graphene is finally prepared, meanwhile, a porous structure and a three-dimensional structure are formed by gas escaping in the processing process, and the controllable three-dimensional patterned graphene blackbody material can be prepared by controlling the laser scanning path and parameters. The surface porous and three-dimensional micro-nano structure of the laser-induced three-dimensional porous graphene black body is beneficial to enhancing the absorption of incident sunlight and improving the photo-thermal conversion efficiency. In addition, after the surface functionalization treatment, the surface hydrophilicity is increased, and the water adsorption capacity can be enhanced. The graphene blackbody material prepared by laser enhances optical absorption, realizes high-efficiency photo-thermal conversion, is used for solar seawater desalination, photo-thermal enhancement photocatalysis and electrocatalysis, and can also be used as a supercapacitor electrode material.
The invention is realized by the following technical scheme:
a preparation method of a three-dimensional patterned porous graphene blackbody is characterized in that short pulse laser is adopted to directly irradiate a carbonaceous material, photons interact with electrons of the carbonaceous material to generate impact ionization and electron-lattice energy transfer, part of carbon is gasified to form a cavity, and the rest of carbon forms a network three-dimensional blackbody-like structure.
The short pulse laser is nanosecond or femtosecond laser.
The carbon material is various carbon materials prepared by carbonization, activation and molding treatment of molded biomass porous carbon, carbonaceous sponge, film, gel and the like.
Further, the preparation method comprises the following steps:
after ultrasonic cleaning is carried out on the carbonaceous material, the carbonaceous material is fixed on a substrate, and the relative position of the carbonaceous material and a short pulse laser source is adjusted to enable laser to be focused on the surface of the carbonaceous material or to be properly defocused;
setting a laser processing program to perform laser processing, so that part of the carbonaceous material is gasified instantly under the action of laser, the rest part forms a network-shaped three-dimensional blackbody-like structure, and simultaneously, the unvaporized carbon material is directly converted into crystalline graphene by a local thermal field of the laser, namely, the laser-induced porous graphene blackbody with a three-dimensional structure and patterning is obtained on the surface layer.
Preferably, the method further comprises a surface functional group modification treatment:
and performing surface hydrophilic/hydrophobic modification treatment on the prepared three-dimensional patterned porous graphene black body by using laser. For example, the three-dimensional patterned porous graphene black body is provided with hydrophilic groups (-PhSO) 3 H) Can be obtained by impregnating a solution of sulfanilic acid and sodium nitrite at 60 ℃ under the protection of nitrogen. Also, a three-dimensional patterned porous graphene-like black body having a hydrophobic property can be obtained by impregnating an acetonitrile solution containing pentafluorophenyl and amyl nitrite under nitrogen protection and heating to 60 ℃ for 24 hours.
Further, fixing the biomass-molded porous carbon, the carbonaceous sponge, the gel, the film and the like on a flat substrate by using a fixing tool, wherein the fixing tool comprises but is not limited to adhesive tapes, glue and the like, and the flat substrate comprises but is not limited to glass, an acrylic plate, a steel plate and the like; the laser focusing position is the upper surface of the carbon material, and the vertical distance between the laser lens and the upper surface of the processed carbon material is 6-6.5 cm; setting parameters such as power, scanning path and the like in laser control software, and obtaining the porous graphene blackbody material after laser processing.
The invention further aims to provide an application of the porous graphene blackbody material with the three-dimensional pattern prepared by using a laser processing method in sea water desalination, photo-thermal enhancement catalysis, super-capacitors and other aspects.
Compared with the prior art, the invention has the following advantages:
(1) The nano-microstructure processing is carried out on the formed carbonaceous material by utilizing the short pulse laser, the interaction between the laser and carbon can be utilized to generate the interaction between light, electrons and phonons, the direct sublimation gasification rather than the hot melting phenomenon of the raw materials with wide sources can be realized, the graphene conversion can be simultaneously carried out, and the method has the advantages of no need of a catalyst, no toxicity, no contact and the like, and is simple in process and low in cost.
(2) The three-dimensional patterned porous graphene blackbody material prepared by short pulse laser induction has a loose porous structure and a three-dimensional nano-microstructure, so that blackbody-like characteristics are realized, the specific surface area of the material is remarkably increased, the internal conduction path of sunlight is increased, and the sunlight absorption and light-heat conversion utilization rate is enhanced;
(3) The short pulse laser induced three-dimensional patterned porous graphene black body can be reused, is environment-friendly and convenient to store and transport;
(4) The laser-induced three-dimensional patterned porous graphene blackbody has strong adaptability and can be processed and prepared according to actual needs.
(5) The invention utilizes the interaction between the short pulse laser and the carbon material to generate the action of light, electrons and phonons instead of the hot melting process, and carries out fine nano-micro structure processing on the surface of the carbon material to realize the graphene black body structure.
Drawings
Fig. 1 is a schematic diagram of a preparation flow of a three-dimensional patterned porous graphene black body (nano-microstructure) prepared by a processing method using a short pulse laser direct gasification mode.
Fig. 2 is a photograph of a three-dimensional patterned porous graphene black body prepared by a short pulse laser processing method according to the present invention after processing a biomass molded porous carbon and a carbonaceous film. The patterns in the left graph are SIOM (scale integrated optical modeling) for the Shanghai ray machine, and the black square areas in the right graph are processed three-dimensional porous graphene black bodies.
FIG. 3 is a Raman spectrum image of porous graphene prepared by a preparation method of a three-dimensional patterned porous graphene blackbody prepared by a short pulse laser processing method; in the figure, the laser-induced three-dimensional porous graphene black body (LMPC) has obvious 2D peaks and the like, and is proved to be completely converted into graphene (wherein MPC is a molded carbon material which is not subjected to laser processing).
Fig. 4 is a scanning electron microscope image of porous graphene prepared by a preparation method of a three-dimensional patterned porous graphene black body prepared by a short pulse laser processing method. The left graph is graphene (scanning electron microscope picture) of the three-dimensional micro-nano structure array; the right panel shows the graphene porous structure (transmission electron microscopy picture).
Fig. 5 shows that the porous graphene blackbody structure prepared by the preparation method of the three-dimensional patterned porous graphene blackbody prepared by the short pulse laser processing method of the invention remarkably improves the light absorptivity.
FIG. 6 shows a three-dimensional patterned porous graphene black body prepared by a method for preparing a porous graphene black body by a short pulse laser processing method for sea water desalination; the left diagram is a schematic diagram of the device; the right graph shows the salt removal effect.
Fig. 7 shows a method for preparing a three-dimensional patterned porous graphene black body by using a short pulse laser processing method, wherein the porous graphene black body is applied to catalytic degradation of an organic dye.
Fig. 8 is an application of a porous graphene black body prepared by a preparation method of a three-dimensional patterned porous graphene black body prepared by a short pulse laser processing method in the aspect of a super capacitor.
Detailed Description
The following describes specific embodiments of the present invention in detail with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
Example 1
The commercial laser used in the invention can be a nanosecond laser, a picosecond laser, a femtosecond laser and the like, and the carbon material comprises but is not limited to formed biomass porous carbon, carbonaceous sponge, foam, gel, film and the like, wherein the biomass porous carbon is a carbon material prepared by biomass such as plant straw, fruit shell and the like, and comprises but is not limited to porous carbon, mesoporous carbon, coal, active carbon and the like.
The preparation method of the three-dimensional patterned porous graphene black body prepared by using the short pulse laser induction processing method comprises the following specific steps:
(1) Inducing by using a laser processing technology to obtain a porous graphene blackbody: processing the molded carbon material into a disc shape with a diameter of 30 mm, and then fixing the disc-shaped carbon material on a substrate by using a fixing device, wherein the fixing device comprises, but is not limited to, an adhesive tape, a clamping tool and the like; planarizing substrates include, but are not limited to: glass, acrylic plates, wood plates, metal plates, and the like. And adjusting the relative position of the substrate and the laser head to enable the laser spot to be in a region to be processed, wherein the focus is at or slightly higher than the upper surface of the carbon material to be processed, namely in a focusing or micro-defocusing state. The laser engraving power is adjusted to 5-100W, the scanning speed is 200-5000 mm/s, and the scanning path such as a circle or letter and other arbitrary shapes are input in software. As shown in fig. 1, after laser irradiation, the carbonaceous material absorbs energy and generates free electrons under the action of a short pulse laser, ionization occurs, part of carbon is directly converted, and the rest of carbon generates heat balance between electrons and crystal lattice, so that the carbon with an amorphous structure is directly converted into a porous graphene blackbody material with three-dimensional stereo patterning.
(2) And (3) performing surface hydrophilic/hydrophobic treatment on the laser-induced three-dimensional porous graphene black body prepared in the step (1) by using chemical functional group modification treatment. Dipping solution of sulfanilic acid and sodium nitrite at 60 ℃ under the protection of nitrogen to obtain hydrophilic group (-PhSO) 3 H) Is black in shape. Also, an acetonitrile solution containing pentafluorophenyl and amyl nitrite was immersed under nitrogen protection and heated to 60 ℃ for 24 hours to obtain a three-dimensional patterned porous with hydrophobic groups on the surfaceGraphene-like blackbody material.
FIG. 1 is a schematic diagram of the preparation process of the present invention, wherein the preparation process is simple and does not require complex processing; FIG. 2 is a left diagram of a SIOM image prepared according to a preset laser scanning path, wherein the SIOM part is completely converted into graphene, and a black area in the center of the right diagram of FIG. 2 is a patterned porous graphene black body prepared by scanning a carbon film with laser; as can be seen from fig. 3, the characteristic peak positions of the coating after processing are consistent with those of graphene, which indicates that the porous carbon material has been completely converted into graphene; from fig. 4, it can be seen that graphene is a three-dimensionally patterned porous blackbody-like structure; fig. 5 is a graph of the absorption performance of graphene black body microstructures to sunlight, and after laser processing, the graphene structures are concave-convex three-dimensional microstructures, so that the optical absorption performance is remarkably improved.
Example 2
As shown in fig. 6, an application of a hydrophilic porous graphene black body prepared by a laser processing method in sea water desalination, specifically, a container with a dome and a diameter of 8 cm is used as a fresh water collecting device; coating hydrophilic materials such as hydrophilic fiber cloth on the surface of cylindrical heat insulation foam, and placing the cylindrical heat insulation foam in a circular plastic beaker with the diameter of 5 cm and containing water to be treated; the hydrophilic porous graphene blackbody material prepared by the method is processed into a round shape with the diameter of 5 cm, so that the round shape is in decryption contact with hydrophilic fiber cloth; under the irradiation of sunlight, the porous graphene black body absorbs light, converts the light into heat, heats and evaporates water absorbed by the hydrophilic fiber cloth at the bottom, and the heat-insulating foam plays a role in heat management, so that sea water desalination, sewage treatment and the like are realized. The vapor condenses in the dome container and collects and flows into other storage devices.
The principle of the invention is that the interaction between laser and carbon atoms is utilized to generate non-hot melting processes such as electron stimulated ionization, electron phonon coupling, lattice thermal vibration and the like, so that carbonaceous materials are gasified instantly to form a large number of three-dimensional patterned three-dimensional micro-nano structures, and graphitization transformation is generated at the same time, and loose and porous graphene black bodies are induced to generate under the irradiation of laser. The graphene black body structure in the porous state is beneficial to increasing the propagation path of incident light, and the optical absorptivity is remarkably improved. In addition, the graphene has good photo-thermal conversion capability and heat conduction performance, and has good treatment effect in sea water desalination and other aspects in addition to the hydrophilic characteristic.
Example 3
As shown in fig. 7, an application of a three-dimensional patterned porous graphene blackbody prepared by a short pulse laser processing method in terms of photo-thermal catalysis and photo-catalytic degradation of organic matters is specifically to place a laser-induced three-dimensional patterned graphene blackbody material with a size of 1*1 cm as a working electrode in a circular plastic beaker with a diameter of 5 cm, which is filled with organic wastewater to be treated; the method adopts a two-electrode system, takes graphite as a counter electrode, and enhances the electrochemical catalytic degradation of organic matters by illumination.
The principle of the invention is that the graphitized transformation is generated by utilizing the laser to induce the carbon material, and the generation of the graphene black body is induced under the irradiation of the laser, and in the whole process, part of carbon is gasified to form a large amount of porous structures. The graphene black body with the characteristics of porous and three-dimensional structures is beneficial to increasing the specific surface area, enhancing the light absorption and the photo-thermal conversion and remarkably improving the catalytic degradation effect.
Example 4
The application of a three-dimensional patterned porous graphene black body prepared by a short pulse laser processing method in the aspect of a super capacitor, specifically, a laser-induced three-dimensional patterned graphene material with a size of 1*1 cm is used as a working electrode to be placed in a circular beaker with a diameter of 5 cm and filled with KOH solution; and a three-electrode system is adopted, pt is used as a counter electrode, and a calomel electrode is used as a reference electrode, so that the capacitance performance of the capacitor is tested. The principle of the invention is that the laser is utilized to induce the carbon material to generate three-dimensional patterning porous graphitized micro-nano blackbody structure transformation, the specific surface area is obviously improved, and the conductivity is improved. The graphene blackbody structure in a porous state is beneficial to increasing the reaction and exchange rate of ions, and the performance of the capacitor is obviously improved.
The three-dimensional patterned porous graphene blackbody disclosed by the invention is a porous graphene material with a three-dimensional micro-nano blackbody structure, which is obtained by processing a carbon material (including but not limited to biomass porous carbon, carbonaceous sponge, carbonaceous foam, carbonaceous gel, carbonaceous film, activated carbon, mesoporous carbon, coal and the like) by using a laser. The prepared graphene blackbody material has good effects in the aspects of enhancing light absorption, realizing photo-thermal conversion, interface evaporation, photo-enhanced catalysis, super-capacitor and the like, and can be applied to applications including but not limited to sea water desalination, catalytic degradation, energy supply and the like. In embodiment 2, a graphene blackbody coating prepared by laser is combined with other components, so that a device for local thermal interface evaporation is designed, the device can be applied to the application environment, the graphene blackbody coating effectively improves the absorption of sunlight broad spectrum, and can reach more than 95%, so that light is converted into heat, the thermal localized utilization is realized, evaporation is realized on seawater or sewage adsorbed by capillary action, and finally the purification treatment of water is realized. Embodiment 3 is in the field of photo-enhanced catalytic degradation, and the photo-thermal enhancement of the three-dimensional patterned porous graphene blackbody material is utilized to further improve the catalytic degradation capability, so that the effect can be improved by more than 30%. Embodiment 4 is a three-dimensional patterned porous graphene blackbody structure prepared on the surface of a carbon material by laser, so that the transmission performance of electrons or ions is enhanced, the specific surface area is increased, and the capacitance performance of the original carbon material can be improved by 40%.
The preferred embodiments of the present invention have been described in detail above with reference to the accompanying drawings, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (10)
1. A preparation method of a three-dimensional patterned porous graphene blackbody is characterized in that short pulse laser is adopted to directly irradiate a carbonaceous material, photons interact with electrons of the carbonaceous material to generate impact ionization and electron-lattice energy transfer, so that part of the carbonaceous material is gasified instantly to form a cavity, the rest part forms a network three-dimensional blackbody-like structure, and meanwhile, a local thermal field of the laser enables unvaporized carbon material to be directly converted into crystalline graphene, namely, the laser-induced porous graphene blackbody with a three-dimensional structure and patterning is obtained on a surface layer; the short pulse laser is nanosecond or femtosecond laser.
2. The method for preparing the three-dimensional patterned porous graphene black body according to claim 1, wherein the carbon material is a formed biomass porous carbon, a carbonaceous sponge, a film and a gel, and is prepared by carbonization, activation and forming treatment.
3. The method for preparing the three-dimensional patterned porous graphene black body according to any one of claims 1 to 2, which is characterized by comprising the following steps:
after ultrasonic cleaning is carried out on the carbonaceous material, the carbonaceous material is fixed on a substrate, and the relative position of the carbonaceous material and a short pulse laser source is adjusted to enable laser to be focused on the surface of the carbonaceous material or to be properly defocused;
setting a laser processing program to perform laser processing, so that part of the carbonaceous material is gasified instantly under the action of laser, the rest part forms a network-shaped three-dimensional blackbody-like structure, and simultaneously, the unvaporized carbon material is directly converted into crystalline graphene by a local thermal field of the laser, namely, the laser-induced porous graphene blackbody with a three-dimensional structure and patterning is obtained on the surface layer.
4. The method of claim 3, wherein the laser focusing position is the upper surface of the carbonaceous material.
5. The method for preparing the three-dimensional patterned porous graphene black body according to claim 1, wherein the parameters and the scanning path of the laser are set, and the laser is focused or properly defocused by 0-10 mm.
6. The method for preparing the three-dimensional patterned porous graphene black body according to claim 1, wherein the laser is nanosecond laser or femtosecond laser short pulse laser, the power is 1-100 watts, and the scanning speed is 100-5000 mm/s.
7. The three-dimensional patterned porous graphene blackbody is characterized by being prepared by the preparation method of the three-dimensional patterned porous graphene blackbody according to any one of claims 1 to 6.
8. The use of a three-dimensional patterned porous graphene-like black body according to claim 7 in ocean freshwater.
9. The use of a three-dimensional patterned porous graphene-like black body according to claim 7 for catalytic degradation of organic dyes.
10. The use of a three-dimensional patterned porous graphene-like blackbody according to claim 7 in a supercapacitor.
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