CN114614029A - Preparation method of integrated air electrode loaded with ultrafine metal nanoparticles - Google Patents
Preparation method of integrated air electrode loaded with ultrafine metal nanoparticles Download PDFInfo
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- 239000002082 metal nanoparticle Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical class C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims abstract description 30
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical class [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 11
- 239000000839 emulsion Substances 0.000 claims abstract description 11
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 11
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 11
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000007731 hot pressing Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 23
- 239000002002 slurry Substances 0.000 claims description 17
- 239000011248 coating agent Substances 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000002243 precursor Substances 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 8
- 229910052723 transition metal Inorganic materials 0.000 claims description 7
- -1 transition metal salt Chemical class 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 claims description 4
- 239000006230 acetylene black Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000001771 vacuum deposition Methods 0.000 claims description 4
- 229910021577 Iron(II) chloride Inorganic materials 0.000 claims description 3
- 239000012018 catalyst precursor Substances 0.000 claims description 3
- 239000004744 fabric Substances 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(II) nitrate Inorganic materials [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 45
- 230000003197 catalytic effect Effects 0.000 abstract description 12
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 239000002184 metal Chemical class 0.000 abstract description 7
- 239000002923 metal particle Substances 0.000 abstract description 7
- 239000011229 interlayer Substances 0.000 abstract description 4
- 150000003839 salts Chemical class 0.000 abstract description 4
- 150000001298 alcohols Chemical class 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 28
- 239000000243 solution Substances 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000007784 solid electrolyte Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 229910017061 Fe Co Inorganic materials 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8828—Coating with slurry or ink
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8875—Methods for shaping the electrode into free-standing bodies, like sheets, films or grids, e.g. moulding, hot-pressing, casting without support, extrusion without support
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9041—Metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
Abstract
The invention provides a preparation method of an integrated air electrode loaded with superfine metal nano particles, which directly mixes pyrrole, ammonium persulfate, metal salt, conductive carbon black, PTFE emulsion and alcohols to form a microporous layer with good catalytic performance, the pyrrole, the ammonium persulfate and the metal salt react to ensure that the formed metal particles are about 2 to 3nm, the superfine metal nano particles have high specific surface area and uniform dispersity, and finally the integrated air electrode is prepared by hot pressing and sintering, a catalytic layer is directly cancelled, and the interlayer contact resistance is reduced. In addition, the dispersion of the ultrafine metal particles in the microporous layer can reduce the resistivity on the premise of ensuring that the porosity is not influenced, thereby improving the performance of the zinc-air battery.
Description
Technical Field
The invention relates to a preparation method of an air electrode for a zinc-air battery, in particular to a preparation method of an integrated air electrode loaded by ultrafine metal nanoparticles.
Background
The air electrode of the zinc-air battery is prepared mainly by coating, rolling or spraying catalyst slurry on the microporous layer to prepare a catalyst layer, so that a three-layer structure comprising the catalyst layer, the microporous layer and the carbon fiber substrate is formed from top to bottom, the air electrode prepared by the method needs to be coated layer by layer, the interlayer contact resistance is large, the gas transmission capability of a diffusion layer can be influenced to a certain extent by coating the catalyst layer, and the preparation of the air electrode is mainly divided into two ways of a wet method and a dry method at present:
according to the invention patent CN201110174416.1, the catalyst is mixed with ethanol and PTFE emulsion to form catalyst layer slurry, and then the catalyst layer slurry is folded and rolled for multiple times, so that the catalyst layer reaches the specified thickness to form the required air electrode. In patent CN201810646499.1, the catalyst, the conductive powder and the binder are directly and uniformly mixed according to a certain mass ratio, then the mixture is directly rolled into a catalytic layer film, and the catalytic layer film is pressed on the microporous layer. The air electrode prepared by the two methods has more layers and large interlayer contact resistance, and the conductivity of the air electrode is influenced.
The invention patent CN201810215133.9 discloses a preparation method of a catalyst and an air battery, which is to prepare the catalyst with the diameter of 5nm-50 μm under the action of plasma flow, mix the catalyst with a carbon material and a binder to prepare catalyst layer slurry, and perform tabletting to prepare a membrane and then coat the membrane on a microporous layer. The catalytic material formed by the preparation method has larger particle size and small specific surface area, influences the gas transmission of the microporous layer and has limited improvement on the catalytic performance.
Therefore, under the condition of ensuring the service life of the battery, the preparation process of the air electrode is simplified, the three-layer structure is simplified into two layers, the integrated air electrode with the catalytic performance is prepared, and the interface contact resistance is further reduced. And the catalyst is loaded by small particles with the diameter of 2-3nm, so that the catalytic capacity can be improved on the premise of not influencing the porosity, and the oxygen transmission capacity of the air electrode and the battery performance are improved.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of an integrated air electrode loaded with ultrafine metal nanoparticles, wherein ultrafine metal particles are dispersed in microporous layer slurry to directly prepare a microporous layer with catalytic performance, so that the integrated air electrode with catalytic performance is further formed, and the ultrafine metal nanoparticles have no porosity while enhancing the conductivity of the microporous layer, so that gas transmission is ensured, the battery performance can be effectively improved, and the integration of the air electrode of a zinc-air battery is facilitated.
The invention is realized by the following technical scheme: the preparation method of the integrated air electrode loaded with the ultrafine metal nanoparticles is characterized by comprising the following steps of:
step A, preparing a microporous layer precursor loaded by ultrafine metal nanoparticles;
step B, coating a microporous layer;
and step C, preparing an integrated air electrode.
As a preferred implementation mode, the method comprises the following specific steps: mixing transition metal salt and conductive carbon black, directly stirring the mixture and pyrrole solution containing ammonium persulfate to react, washing the mixture to be neutral, and stirring and mixing the mixture with 20% PTFE emulsion and alcohol solution to prepare microporous layer slurry containing a catalyst precursor;
coating the prepared microporous layer slurry on a carbon paper or carbon cloth substrate, and naturally drying to obtain an electrode precursor;
and pressing the electrode precursor under a hot press, and then sintering at high temperature under the protection of inert gas to obtain the integrated air electrode loaded with the superfine metal nanoparticles.
After the technical scheme is adopted, the invention has the beneficial effects that: pyrrole, ammonium persulfate and metal salt are directly mixed with conductive carbon black, PTFE emulsion and alcohols to form a microporous layer with good catalytic performance. Pyrrole and ammonium persulfate react with metal salt to ensure that the formed metal particles are about 2-3nm, the superfine metal nanoparticles have high specific surface area and uniform dispersity, and finally an integrated air electrode is prepared by hot pressing and sintering, so that a catalyst layer is directly omitted, and the interlayer contact resistance is reduced. In addition, the dispersion of the ultrafine metal particles in the microporous layer can reduce the resistivity on the premise of ensuring that the porosity is not influenced, thereby improving the performance of the zinc-air battery.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic view of an air electrode according to the present invention, compared with a conventional air electrode.
FIG. 2 is a scanning electron microscope photograph of the cross section, the lower bottom surface (carbon paper substrate) and the upper surface (microporous layer containing ultrafine metal particles) of the integrated air electrode in example 1 of the present invention;
FIG. 3 is a transmission electron microscope image and particle size distribution of Fe-Co metal particles in the integrated air electrode loaded with ultrafine metal nanoparticles of example 1;
FIG. 4 is a table comparing the porosity and resistivity of the 3 air electrodes of examples 1-3;
FIG. 5 is a graph comparing polarization curves of 3 air electrodes in examples 1-3.
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 derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a technical scheme that: the preparation method of the integrated air electrode loaded with the ultrafine metal nanoparticles is characterized by comprising the following steps of:
step A, preparing a microporous layer precursor loaded by ultrafine metal nanoparticles;
step B, coating a microporous layer;
and step C, preparing an integrated air electrode.
The method comprises the following specific steps: mixing transition metal salt and conductive carbon black, directly stirring the mixture and pyrrole solution containing ammonium persulfate to react, washing the mixture to be neutral, and stirring and mixing the mixture with 20% of PTFE emulsion and alcohol solution to prepare microporous layer slurry containing a catalyst precursor;
coating the prepared microporous layer slurry on a carbon paper or carbon cloth substrate, and naturally drying to obtain an electrode precursor;
and pressing the electrode precursor under a hot press, and then sintering at high temperature under the protection of inert gas to obtain the integrated air electrode loaded with the ultrafine metal nanoparticles.
In the step A, the volume ratio of pyrrole to water in the pyrrole solution is 1: 75-80, wherein the mass ratio of ammonium persulfate to pyrrole solution is 1: 30, the mass ratio of the transition metal salt to the conductive carbon black is 1: 5, the mass concentration of the PTFE emulsion is 10 percent.
The transition metal salt in the step A adopts CoCl2，FeCl2，Ni(NO3)2One or more of them.
The type of the conductive carbon black in the step A is one of acetylene black, XC-72, XC-72R, EC-600 and EC-300.
In the step A, the alcohol is one of isopropanol, ethanol, ethylene glycol and methanol.
The coating thickness of the vacuum coating in the step B is 20-100 um.
In the step C, the hot-pressing condition of the hot press is 130-160 ℃, and the pressure is 1.5-2.5 Mpa. The sintering temperature is 700-1000 ℃, and the sintering time is 1.5-3 h.
As an embodiment of the present invention:
the first embodiment is as follows:
zinc-air battery with integrated air electrode loaded with ultra-fine metal nanoparticles:
0.5g FeCl was weighed2And 0.5g CoCl2And 5g of acetylene black, adding the mixture into 30ml of deionized water containing 400ul of pyrrole, adding 1g of ammonium persulfate, mixing and stirring to obtain a mixed solution a, washing to be neutral, and directly mixing and stirring with 8g of 10% PTFE emulsion and 200g of isopropanol to obtain slurry b.
And coating the slurry b on a carbon paper substrate through a vacuum coating machine, wherein the coating thickness is 50um, and naturally airing to obtain the air electrode precursor.
And (3) carrying out hot pressing on the prepared air electrode precursor for 5 minutes under a hot press (160 ℃ and 2 Mpa). And then sintering the substrate for 2 hours at 800 ℃ in argon to obtain the integrated air electrode loaded with the ultrafine metal nanoparticles.
And assembling the integrated air electrode loaded with the ultrafine metal nanoparticles, the alkaline solid electrolyte and the metal zinc foil negative electrode into a 5 x 5cm solid zinc-air battery.
Example two:
preparing an air electrode containing a conventional catalyst layer containing ultrafine metal nanoparticles:
400ul of pyrrole is dispersed in 30ml of deionized water by ultrasonic, and then 1g of ammonium persulfate is added to be mixed and stirred to obtain a solution a.
The solution a is washed dry and then admixed with 0.5g of CoCl2And 0.5g FeCl2Mixing in deionized water, ultrasonic dispersing for 60min to obtain product b,
and (3) sintering the obtained product b for 2h at 800 ℃ in argon after freeze drying, washing the sample to be neutral, and drying to obtain the catalyst c.
Catalyst c 2g, 8g of 10% PTFE emulsion and 200g of isopropanol were weighed, mixed and stirred to obtain catalyst slurry, and the catalyst slurry was knife-coated on a gas diffusion layer having a microporous layer to a thickness of 50 μm.
And assembling the air electrode containing the non-noble metal catalyst layer, the alkaline solid electrolyte and the metal zinc foil cathode into a 5 x 5cm solid zinc-air battery.
Example three:
a zinc-air battery prepared from an air electrode without catalyst loading:
6g of acetylene black, 8g of 10% PTFE emulsion and 200g of isopropanol were mixed and stirred to prepare a microporous layer slurry b.
And coating the slurry b on a carbon paper substrate through a vacuum coating machine, wherein the coating thickness is 50um, and naturally airing to obtain the air electrode precursor.
And (3) carrying out hot pressing on the prepared air electrode precursor for 5 minutes under a hot press (160 ℃ and 2 Mpa). Then sintering at 800 ℃ for 2h in argon to obtain the air electrode without catalyst loading.
The air electrode without catalyst load, alkaline solid electrolyte and metal zinc foil negative electrode are assembled into a 5X 5cm solid zinc-air battery.
With reference to figures 1-5.
By comparing examples 1 to 3, it can be found that the integrated air electrode loaded with ultrafine metal nanoparticles in example 1 has lower resistivity without affecting the porosity thereof, and does not need to be additionally coated with a catalyst layer, and the integrated air electrode has simple process and excellent performance.
By comparing example 1 with example 2, it can be seen that the integrated electrode prepared by one-step molding can effectively reduce the conductivity and improve the performance of the zinc-air battery compared with the electrode prepared by preparing the catalyst first and then blade-coating layer by the traditional step method.
By comparing the example 1 with the example 3, the electrode without the metal nanoparticle catalyst has extremely poor catalytic performance, and further illustrates that the integrated electrode successfully and effectively combines the catalyst with the electrode preparation process, thereby improving the electrode performance.
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 (8)
1. The preparation method of the integrated air electrode loaded with the ultrafine metal nanoparticles is characterized by comprising the following steps of:
step A, preparing a microporous layer precursor loaded by ultrafine metal nanoparticles;
step B, coating a microporous layer;
and step C, preparing an integrated air electrode.
2. The method of claim 1, wherein the method comprises the following steps: the method comprises the following specific steps: mixing transition metal salt and conductive carbon black, directly stirring the mixture and pyrrole solution containing ammonium persulfate to react, washing the mixture to be neutral, and stirring and mixing the mixture with 20% of PTFE emulsion and alcohol solution to prepare microporous layer slurry containing a catalyst precursor;
coating the prepared microporous layer slurry on a carbon paper or carbon cloth substrate, and naturally drying to obtain an electrode precursor;
and pressing the electrode precursor under a hot press, and then sintering at high temperature under the protection of inert gas to obtain the integrated air electrode loaded with the superfine metal nanoparticles.
3. The method of claim 2, wherein the method comprises the following steps: in the step A, the volume ratio of pyrrole to water in the pyrrole solution is 1: 75-80, wherein the mass ratio of ammonium persulfate to pyrrole solution is 1: 30, the mass ratio of the transition metal salt to the conductive carbon black is 1: 5, the mass concentration of the PTFE emulsion is 10 percent.
4. The method of claim 1, wherein the method comprises the following steps: the transition metal salt in the step A adopts CoCl2，FeCl2，Ni(NO3)2One or more of them.
5. The method of claim 4, wherein the method comprises the following steps: the type of the conductive carbon black in the step A is one of acetylene black, XC-72, XC-72R, EC-600 and EC-300.
6. The method of claim 5, wherein the method comprises the following steps: in the step A, alcohol is selected from isopropanol, ethanol, glycol and methanol.
7. The method of claim 1, wherein the method comprises the following steps: the coating thickness of the vacuum coating in the step B is 20-100 um.
8. The method of claim 1, wherein the method comprises the steps of: and C, the hot-pressing condition of the hot press in the step C is 130-160 ℃, the temperature is 1.5-2.5Mpa, the sintering temperature is 700-1000 ℃, and the sintering time is 1.5-3 h.
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