CN107799314B - Molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane and preparation method thereof - Google Patents
Molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane and a preparation method and application thereof, and belongs to the technical field of flexible solar cells. The composite nanofiber membrane is used as a counter electrode, the titanium carbide/carbon composite nanofiber membrane is used as a carrier, and molybdenum disulfide is loaded on the titanium carbide/carbon composite nanofiber membrane carrier through a sintering method to prepare the composite nanofiber membrane. The invention adopts a simple sintering method to realize MoS 2 Combined with TiC/C flexible composite nanofiber membrane and MoS 2 Evenly distributed on the surface of the nanofiber, and greatly improves the electrocatalytic performance of the composite nanofiber membrane while not damaging the flexibility of the composite nanofiber membrane. Namely, the preparation of the composite nanofiber membrane electrode with high flexibility and high catalytic activity is realized. Based on the pair of electrodes, the high-efficiency high-flexibility DSSC is assembled, so that the DSSC has the potential of being combined with textiles, and the application of the DSSC is greatly widened and the development of photovoltaic intelligent textiles is promoted.
Description
Technical Field
The invention relates to a molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane and a preparation method and application thereof, and belongs to the technical field of flexible solar cells.
Background
With the development of science and technology, intelligent textiles are gradually appeared in our field of vision, and the rise of the emerging industry is a great progress in human society. And the intelligent textile based on the battery is an important direction of the textile and is also a key factor for restricting the wearable electronic product. Solar cells that convert inexhaustible solar energy into electrical energy are favored by vast researchers. However, it is a hot spot of research how conventional solar cells are relatively rigid, and how to make the solar cells meet wearable requirements.
Among the solar cells, dye-sensitized solar cells (Dye-Sensitized Solar Cells, DSSC) have the advantages of simple manufacture, readily available materials, low cost and the like. Such cells were taught by M.Gratzel since 1991 using nanoporous TiO with high specific surface area 2 Instead of the conventional flat electrode, an optical transparent film with a thickness of about 10 μm is formed, and then a dye is impregnated, so that the photoelectric conversion efficiency thereof reaches 7.1%. However, conventional DSSCs, because both the photoanode and the counter electrode substrate are glass, result in heavy cell quality, fragile, severely limiting their practical application. If the DSSC can be prepared on a light high-flexibility substrate, the high-flexibility DSSC can be obtained, has the potential of combining with textiles, and greatly promotes the application of the DSSC. The core of the design of the high-flexibility substrate is a photo-anode and a counter electrode, so that the research of the high-flexibility photo-anode is more and has advanced to a certain extent at present, but the research of the high-flexibility counter electrode needs to be further enhanced.
The counter electrode is an important component of the dye sensitized solar cell and is used for collecting electrons of an external circuit and collecting I in electrolyte 3 - Reduction to I - . Conventional counter electrodes are generally composed of platinized conductive glass, however, platinum materials are costly and long-termIs easy to be corroded by electrolyte. In recent years, the carbon material has the characteristics of good electrical conductivity, thermal conductivity, catalytic activity and corrosion resistance, and has wide development prospect in the application field of the counter electrode. Accordingly, carbon material counter electrodes such as graphene thin film counter electrodes, carbon nanotube thin film counter electrodes, and carbon black thin film counter electrodes have been widely studied. Although these carbon material counter electrodes can effectively reduce the cost of DSSCs, their own preparation process is complex, the yield is low, and the bonding with the counter electrode substrate is difficult, and the stability of the battery is still to be improved, so that the practical application thereof is limited to a certain extent.
In recent years, carbon nanofibers produced by electrospinning have attracted more and more attention as DSSCs counter electrodes. Carbon nanofibers and hollow carbon nanofibers are deposited on a conductive glass substrate as counter electrodes for application to DSCSs, respectively, as Qiao et al and Lee et al. Subsequently, qiao et al will TiO 2 The mixed deposition of the nano particles and the carbon nano fibers on the conductive glass substrate is applied to DSSCs. However, because electrospun pure carbon nanofiber membranes are low in strength and brittle, they are difficult to bond to flexible substrates and are generally only applicable to DSSCs on glass substrates. How to obtain a highly flexible and efficient counter electrode is one of the key problems of a highly flexible DSSC.
Disclosure of Invention
The invention aims at solving the problems in the prior art and provides a high-flexibility molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane with good electrocatalytic activity and charge transmission capability.
The aim of the invention can be achieved by the following technical scheme: the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane takes the titanium carbide/carbon composite nanofiber membrane as a carrier, and the molybdenum disulfide is loaded on the titanium carbide/carbon composite nanofiber membrane carrier.
Although the addition of titanium carbide to the carbon nanofiber membrane can significantly improve the flexibility and electrocatalytic activity of the carbon nanofiber membrane to a certain extent, the electrocatalytic activity is still difficult to compare favorably with that of a platinum electrode. And molybdenum disulfide is a counter electrode material with high catalytic activity. Therefore, the invention combines molybdenum disulfide with the flexible titanium carbide/carbon composite nanofiber membrane, and remarkably improves the electrocatalytic activity of the flexible nanofiber membrane electrode, thereby improving the photoelectric conversion efficiency of the flexible DSSCs.
The second object of the present invention is to provide a preparation method of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane, which comprises the following steps: the titanium carbide/carbon composite nanofiber membrane is used as a carrier, and molybdenum disulfide is loaded on the titanium carbide/carbon composite nanofiber membrane carrier through a sintering method.
In the preparation method of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane, the preparation method of the titanium carbide/carbon composite nanofiber membrane comprises the following steps:
a. preparing a mixed solution of a mixed polymer containing PVP (polyvinylpyrrolidone), PAN (polyacrylonitrile) and PMMA (polymethyl methacrylate) in an organic solvent;
b. adding a catalyst and TiP (isopropyl titanate) into the prepared mixed solution, and preparing the TiP/PVP/PAN/PMMA composite nanofiber membrane by an electrostatic spinning method;
c. pre-oxidizing the prepared TiP/PVP/PAN/PMMA composite nanofiber membrane for 1-4 hours, and carbonizing for 0.5-2 hours under the protection of inert gas to obtain the titanium carbide/carbon composite nanofiber membrane.
In the preparation method of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane, the mass fraction of the mixed polymer of PVP, PAN, PMMA in the mixed solution in the step a is 9-22%.
In the preparation method of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane, the dosage of the catalyst in the step b is 3-10% of the volume of the mixed solution, and the catalyst is preferably glacial acetic acid.
In the preparation method of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane, the amount of the TiP in the step b is 0.2-1.5 times of the mass of the mixed polymer of PVP, PAN, PMMA.
In the preparation method of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane, the pre-oxidation temperature in the step c is 200-300, and the carbonization temperature at the temperature of 900-1200. DEG C
In the preparation method of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane, the specific process of the sintering method is as follows: sintering the titanium carbide/carbon composite nanofiber membrane and molybdenum trisulfide for 3-10 hours at a constant temperature of 400-800 ℃ under the protection of inert gas. The dosage ratio of the molybdenum trisulfide to the titanium carbide/carbon composite nanofiber membrane is any ratio, so that the mass ratio of the prepared molybdenum disulfide to the titanium carbide/carbon composite nanofiber membrane carrier is also any ratio.
A third object of the present invention is to provide an application of the above molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane, which is used as a counter electrode.
In the application of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane, the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane is used as a counter electrode of a dye-sensitized solar cell.
Compared with the prior art, the invention realizes MoS by adopting a simple sintering method 2 Combined with TiC/C flexible composite nanofiber membrane and MoS 2 Evenly distributed on the surface of the nanofiber, and greatly improves the electrocatalytic performance of the composite nanofiber membrane while not damaging the flexibility of the composite nanofiber membrane. Namely, the preparation of the composite nanofiber membrane electrode with high flexibility and high catalytic activity is realized. Based on the pair of electrodes, the high-efficiency high-flexibility DSSC is assembled, so that the DSSC has the potential of being combined with textiles, and the application of the DSSC is greatly widened and the development of photovoltaic intelligent textiles is promoted.
Drawings
FIG. 1 is a FESEM photograph of a molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane prepared in example 1, with the upper right corner being an enlarged view of the nanofiber;
FIG. 2 is a TEM (a) and HRTEM (b-c) photograph of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane prepared in example 1;
FIG. 3 is an XRD pattern of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane prepared in example 1;
FIG. 4 is an XPS full view (a), mo 3d (b) and S2p spectrum (c) of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane prepared in example 1.
FIG. 5 is a schematic view of the flexibility of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane prepared in example 1;
FIG. 6 is a CV curve (a), an EIS spectrum (b) and a Tafel curve (c) of a counter electrode of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane prepared in example 1;
FIG. 7 is a digital photograph of a flexible DSSC (a) and an I-V characteristic curve (b) of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane prepared in example 1 assembled to an electrode.
Detailed Description
The following are specific embodiments of the present invention, and the technical solutions of the present invention will be further described with reference to the accompanying drawings, but the present invention is not limited to these embodiments.
Example 1:
0.28g of PAN, 0.28g of PVP and 0.56g of PMMA are added into 6mL of DMF solvent to form a solution with the mass ratio of 1:1:2:20, after magnetic stirring for 4h, 0.3mL of glacial acetic acid and 0.7mL of isopropyl titanate are added into the solution, and after magnetic stirring for 12h, precursor spinning solution is obtained. And filling the precursor spinning solution into a syringe, controlling the syringe to form jet trickles under the action of 15kV voltage at the extrusion rate of 0.8mL/h by a microinjection pump, and directly collecting the jet trickles on a receiving plate in a disordered state to form the TiP/PVP/PAN/PMMA composite nanofiber membrane. And (3) placing the collected TiP/PVP/PAN/PMMA composite nanofiber membrane into a tube furnace for sintering, heating to 250 ℃ at the speed of 5 ℃/min, preserving heat for 1h, heating to 1000 ℃ at the speed of 5 ℃/min under argon atmosphere, preserving heat for 0.5h, and cooling to normal temperature to obtain the high-flexibility titanium carbide/carbon composite nanofiber membrane.
Preparing a mixed solution of sodium molybdate, sodium sulfide, absolute ethyl alcohol and deionized water in a mass ratio of 1:5:5:21, uniformly stirring, slowly adding dilute sulfuric acid (3.6 mol/L) of which the volume ratio is 1.875 times of absolute ethyl alcohol into the uniformly stirred solution, immediately generating brown pasty precipitate, and carrying out suction filtration, washing and drying on the precipitate to obtain brown molybdenum trisulfide powder.
And (3) placing the titanium carbide/carbon composite nanofiber membrane and molybdenum trisulfide powder into a high-temperature tube furnace, heating to 650 ℃ at a speed of 5 ℃/min under the protection of argon atmosphere, and then preserving heat for 4 hours to obtain the flexible molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane.
Fig. 1 is a FESEM photograph of a molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane prepared in this example, and it can be seen that the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane has some burr-like substances in addition to some nanoparticles uniformly distributed thereon. FIG. 2 is a TEM (a) photograph and HRTEM (b and c) photograph of the molybdenum disulfide/titanium carbide/carbon composite nanofiber prepared in this example, and it can be seen that the nanoparticles distributed on the molybdenum disulfide/titanium carbide/carbon nanofiber film have TiC and MoS 2 Whereas the burr shape is MoS 2 . FIG. 3 is an XRD of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane prepared in this example, in FIG. 3, typical MoS was present in comparison with JCPDS No.75-1539 cards and JCPDS No.32-1383 cards 2 And TiC, thereby confirming MoS 2 And the presence of TiC. The XPS patterns (a-c) of FIG. 4 further demonstrate MoS 2 Is present. Fig. 5 is a schematic view of flexibility of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane prepared in this example, and it can be seen that the fiber membrane can be greatly bent, and shows better flexibility.
The prepared molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane can be directly used as a counter electrode, and is assembled with a sensitized flexible photoanode, a quasi-solid electrolyte and a Surlyn 1702 heat packaging film to form a flexible DSSC. Likewise, DSSCs were assembled based on flexible titanium carbide/carbon composite nanofiber membranes (prepared in the manner of this example) and Pt-plated conductive glass counter electrodes.
And testing and analyzing the electrochemical performances of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane counter electrode, the titanium carbide/carbon composite nanofiber membrane counter electrode and the Pt-plated conductive glass counter electrode. Fig. 6 shows Cyclic Voltammetry (CV) curves (a) and Electrochemical Impedance Spectroscopy (EIS) (b) Tafel polarization (Tafel) curves (c) of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane prepared in this example. From the graph, the cathode current density I in CV curve of molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane can be obtained PC 23.38mA cm -2 For a pair ofSeries resistance R of electrodes s 92.71 Ω cm 2 Charge transfer resistor R ct Is 5.23 Ω cm 2 Exchange current density (J 0 ) Is 3.05mA cm -2 . This demonstrates that the electrocatalytic activity of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane is superior to that of the titanium carbide/carbon composite nanofiber membrane counter electrode and the Pt-plated conductive glass counter electrode. But the charge transfer capability is weaker than that of the titanium carbide/carbon composite nanofiber membrane counter electrode and the Pt-coated conductive glass counter electrode.
Respectively taking the prepared molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane, titanium carbide/carbon composite nanofiber membrane and Pt-plated conductive glass as counter electrodes, and sensitized flexible TiO 2 The photoanode, quasi-solid electrolyte and sand Lin Re encapsulation film (Surlyn 1702) were heat sealed to form a flexible DSSC, which was tested and compared for performance differences between the three types of cells. Fig. 7 is a digital photograph and I-V characteristic of a flexible DSSC. The flexible DSSC may be substantially curved. From the I-V curve, the photoelectric conversion efficiency of the flexible DSSC based on the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane is 5.5%, which is improved by about 22% compared with the battery (4.5%) of the counter electrode of the titanium carbide/carbon nanofiber membrane; higher than the efficiency of the Pt/FTO counter electrode cell (4.60%).
Example 2:
0.48g of PAN, 0.24g of PVP and 0.18g of PMMA are added into 6mL of DMF solvent, after magnetic stirring for 4h, 0.3mL of glacial acetic acid and 0.8mL of isopropyl titanate are added into the solution, and after magnetic stirring for 12h, a precursor spinning solution is obtained. And filling the precursor spinning solution into a syringe, controlling the syringe to form jet trickles under the action of 15kV voltage at the extrusion rate of 0.8mL/h by a microinjection pump, and directly collecting the jet trickles on an aluminum foil of a receiving plate in a disordered state to form the TiP/PVP/PAN/PMMA composite nanofiber membrane. Drying the collected TiP/PVP/PAN/PMMA composite nanofiber membrane, then placing the dried TiP/PVP/PAN/PMMA composite nanofiber membrane into a tube furnace for sintering, heating to 210 ℃ at the speed of 1 ℃/min, then preserving heat for 2 hours, heating to 900 ℃ at the speed of 5 ℃/min under argon atmosphere, preserving heat for 2 hours, and cooling to normal temperature to obtain the high-flexibility titanium carbide/carbon composite nanofiber membrane.
Preparing a mixed solution of sodium molybdate, sodium sulfide, absolute ethyl alcohol and deionized water in a mass ratio of 1:5:5:21, uniformly stirring, slowly adding dilute sulfuric acid (3.6 mol/L) of which the volume ratio is 1.875 times of absolute ethyl alcohol into the uniformly stirred solution, immediately generating brown pasty precipitate, and carrying out suction filtration, washing and drying on the precipitate to obtain brown molybdenum trisulfide powder.
And (3) placing the titanium carbide/carbon composite nanofiber membrane and molybdenum trisulfide powder into a high-temperature tube furnace, heating to 400 ℃ at a speed of 5 ℃/min under the protection of argon atmosphere, and then preserving heat for 8 hours to obtain the flexible molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane.
And testing and analyzing the electrochemical performances of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane counter electrode, the titanium carbide/carbon composite nanofiber membrane counter electrode and the Pt-plated conductive glass counter electrode. The prepared molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane, titanium carbide/carbon composite nanofiber membrane and Pt-plated conductive glass are respectively taken as counter electrodes, and sensitized flexible TiO is adopted 2 The photoanode, quasi-solid electrolyte and sand Lin Re encapsulation film (Surlyn 1702) were heat sealed to form a flexible DSSC, which was tested and compared for performance differences between the three types of cells. The procedure and results of characterization and performance testing were similar to those of example 1, with the most critical photoelectric conversion efficiency being 4.8%, which is slightly higher than that of titanium carbide/carbon composite nanofiber membrane counter electrode cells and Pt/FTO counter electrode cells.
Example 3:
0.16g of PAN, 0.24g of PVP and 0.8g of PMMA are added into 6mL of DMF solvent, after magnetic stirring for 4h, 0.3mL of glacial acetic acid and 1.0mL of isopropyl titanate are added into the solution, and after magnetic stirring for 12h, a precursor spinning solution is obtained. And filling the precursor spinning solution into a syringe, controlling the syringe to form jet trickles under the action of 15kV voltage at the extrusion rate of 0.8mL/h by a microinjection pump, and directly collecting the jet trickles on an aluminum foil of a receiving plate in a disordered state to form the TiP/PVP/PAN/PMMA composite nanofiber membrane. Drying the collected TiP/PVP/PAN/PMMA composite nanofiber membrane, then placing the dried TiP/PVP/PAN/PMMA composite nanofiber membrane into a tube furnace for sintering, heating to 300 ℃ at the speed of 2 ℃/min, then preserving heat for 1h, heating to 1200 ℃ at the speed of 5 ℃/min under argon atmosphere, preserving heat for 0.5h, and cooling to normal temperature to obtain the high-flexibility titanium carbide/carbon composite nanofiber membrane.
Preparing a mixed solution of sodium molybdate, sodium sulfide, absolute ethyl alcohol and deionized water in a mass ratio of 1:5:5:21, uniformly stirring, slowly adding dilute sulfuric acid (3.6 mol/L) of which the volume ratio is 1.875 times of absolute ethyl alcohol into the uniformly stirred solution, immediately generating brown pasty precipitate, and carrying out suction filtration, washing and drying on the precipitate to obtain brown molybdenum trisulfide powder.
And (3) placing the titanium carbide/carbon composite nanofiber membrane and molybdenum trisulfide powder into a high-temperature tube furnace, heating to 800 ℃ at a speed of 5 ℃/min under the protection of argon atmosphere, and then preserving heat for 3 hours to obtain the flexible molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane.
And testing and analyzing the electrochemical performances of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane counter electrode, the titanium carbide/carbon composite nanofiber membrane counter electrode and the Pt-plated conductive glass counter electrode. The prepared molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane, titanium carbide/carbon composite nanofiber membrane and Pt-plated conductive glass are respectively taken as counter electrodes, and sensitized flexible TiO is adopted 2 The photoanode, quasi-solid electrolyte and sand Lin Re encapsulation film (Surlyn 1702) were heat sealed to form a flexible DSSC, which was tested to compare the performance differences between the three types of cells. The procedure and results of characterization and performance testing were similar to those of example 1, with the most critical photoelectric conversion efficiency reaching 5.3%.
In view of the numerous embodiments of the present invention, the experimental data of each embodiment is huge and is not suitable for the one-by-one listing and explanation here, but the content of the verification needed by each embodiment and the obtained final conclusion are close. Therefore, the verification contents of each example are not described one by one, and only examples 1 to 3 are used as representative to describe the superiority of the present invention.
The specific embodiments described herein are offered by way of example only to illustrate the spirit of the invention. Various modifications or additions to the described embodiments may be made by those skilled in the art to which the invention pertains or may be substituted in a similar manner without departing from the spirit of the invention or beyond the scope of the appended claims.
Claims (6)
1. The preparation method of the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane is characterized in that the composite nanofiber membrane takes the titanium carbide/carbon composite nanofiber membrane as a carrier, and the molybdenum disulfide is loaded on the titanium carbide/carbon composite nanofiber membrane carrier;
the preparation method comprises the following steps: taking a titanium carbide/carbon composite nanofiber membrane as a carrier, and loading molybdenum disulfide on the titanium carbide/carbon composite nanofiber membrane carrier by a sintering method;
the specific process of the sintering method is as follows: sintering the titanium carbide/carbon composite nanofiber membrane and molybdenum trisulfide for 3-10 hours at a constant temperature of 400-800 ℃ under the protection of inert gas;
the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane is used as a counter electrode of a dye-sensitized solar cell.
2. The method for preparing the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane according to claim 1, wherein the method for preparing the titanium carbide/carbon composite nanofiber membrane comprises the following steps:
a. preparing a mixed solution of a mixed polymer containing PVP, PAN, PMMA in an organic solvent;
b. adding a catalyst and TiP into the prepared mixed solution, and preparing the TiP/PVP/PAN/PMMA composite nanofiber membrane by an electrostatic spinning method;
c. pre-oxidizing the prepared TiP/PVP/PAN/PMMA composite nanofiber membrane for 1-4 hours, and carbonizing for 0.5-2 hours under the protection of inert gas to obtain the titanium carbide/carbon composite nanofiber membrane.
3. The method for preparing the molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane according to claim 2, wherein the total mass fraction of the mixed polymer in the mixed solution PVP, PAN, PMMA in the step a is 9-22%.
4. The method for preparing a molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane according to claim 2, wherein the catalyst in the step b is used in an amount of 3-10% of the volume of the mixed solution.
5. The method for preparing a molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane according to claim 2, wherein the amount of TiP used in the step b is 0.2-1.5 times the mass of the mixed polymer of PVP, PAN, PMMA.
6. The method for preparing a molybdenum disulfide/titanium carbide/carbon composite nanofiber membrane according to claim 2, wherein the pre-oxidation temperature in the step c is 200-300 ℃, and the carbonization temperature is 900-1200 ℃.
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