CN111916290A - Transition metal sulfide/Ti3C2TxMethod for preparing composite material - Google Patents
Transition metal sulfide/Ti3C2TxMethod for preparing composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 26
- -1 Transition metal sulfide Chemical class 0.000 title claims abstract description 24
- 229910009819 Ti3C2 Inorganic materials 0.000 claims abstract description 47
- 239000007864 aqueous solution Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000243 solution Substances 0.000 claims abstract description 25
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 239000011259 mixed solution Substances 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 229910002001 transition metal nitrate Inorganic materials 0.000 claims abstract description 15
- 239000011541 reaction mixture Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000007710 freezing Methods 0.000 claims abstract description 12
- 230000008014 freezing Effects 0.000 claims abstract description 12
- 238000004108 freeze drying Methods 0.000 claims abstract description 10
- 239000006228 supernatant Substances 0.000 claims abstract description 7
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 6
- 238000009777 vacuum freeze-drying Methods 0.000 claims abstract description 5
- VDQVEACBQKUUSU-UHFFFAOYSA-M disodium;sulfanide Chemical compound [Na+].[Na+].[SH-] VDQVEACBQKUUSU-UHFFFAOYSA-M 0.000 claims description 5
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical compound [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(III) nitrate Inorganic materials [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 2
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(II) nitrate Inorganic materials [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 abstract 1
- 239000008367 deionised water Substances 0.000 description 12
- 229910021641 deionized water Inorganic materials 0.000 description 12
- 239000000463 material Substances 0.000 description 8
- 238000009210 therapy by ultrasound Methods 0.000 description 7
- 239000003990 capacitor Substances 0.000 description 6
- 238000005119 centrifugation Methods 0.000 description 6
- 239000007772 electrode material Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacturing & Machinery (AREA)
Abstract
The invention discloses a transition metal sulfide/Ti3C2TxThe preparation method of the composite material comprises the following steps: (1) adding transition metal nitrate into water to obtain transition metal nitrate water solution; (2) mixing Ti3C2TxAdding into water to obtain Ti3C2TxAn aqueous solution; (3) adding an aqueous solution of a transition metal nitrate to Ti3C2TxIn the water solution, uniformly stirring to obtain a mixed solution; (4) mixing Na2Adding S into water to prepare Na2S solution; (5) mixing Na2Adding the S solution into the mixed solution, and stirring until the reaction is complete to obtainTo the reaction mixture; (6) centrifuging the reaction mixture, and removing the supernatant to obtain a turbid sample; (7) freezing the turbid sample; (8) taking out the frozen turbid sample, and freeze-drying in a vacuum freeze-drying machine at low temperature to obtain the transition metal sulfide/Ti3C2TxA composite material. The composite material prepared by the preparation method has large specific surface area of 3 A.g‑1Specific capacitance under current density is up to 768 F.g‑1Simple operation, low cost, rapidness and environmental protection.
Description
Technical Field
The invention relates to a preparation method of a composite material, and more particularly relates to a transition metal sulfide/Ti3C2TxA method for preparing a composite material.
Background
MXene is a novel two-dimensional transition metal carbide (or nitride, carbonitride) and has the advantages of high conductivity, high surface area, stable chemical properties and the like, wherein Ti is used as a main component3C2TxIs a two-dimensional transition metal carbide in MXene family, has extremely large specific surface area, excellent conductivity and good chemical stability, and is very suitable to be used as an electrode material. However, Ti3C2TxThe van der Waals forces between the sheets are so large that they cannot peel off a single-layer or multi-layer structure like graphene, thereby failing to exert Ti3C2TxThe material has the advantage of large specific surface area. Such a disadvantage limits Ti3C2TxThe further development and application of the material in the field of energy storage can improve Ti by compounding with other substances and other methods3C2TxThe electrochemical performance of the material is that the transition metal sulfide has typical metal characteristics, higher specific capacity, thermal stability and mechanical stability, and can be combined with Ti3C2TxThe material is compounded to prepare a novel super capacitor electrode material, so that the high specific capacity of the metal sulfide and Ti are exerted3C2TxHigh conductivity, and can effectively improve the electrochemical performance of the electrode material. However, the existing preparation method is complex and difficult to operate, has high cost and low efficiency, and the prepared composite material has small specific surface area and influences the electrochemical performance.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide transition metal sulfide/Ti with low cost, rapidness, environmental protection and large specific surface area and high specific capacitance of the prepared product3C2TxPreparation of composite materialsThe preparation method is as follows.
The technical scheme is as follows: the transition metal sulfide/Ti of the invention3C2TxThe preparation method of the composite material comprises the following steps:
(1) adding transition metal nitrate into water to obtain transition metal nitrate water solution;
(2) mixing Ti3C2TxAdding into water to obtain Ti3C2TxAn aqueous solution;
(3) adding an aqueous solution of a transition metal nitrate to Ti3C2TxIn the water solution, uniformly stirring to obtain a mixed solution;
(4) mixing Na2Adding S into water to prepare Na2S solution;
(5) mixing Na2Adding the S solution into the mixed solution obtained in the step (3), and stirring until the reaction is complete to obtain a reaction mixture;
(6) centrifuging the reaction mixture in the step 5, and removing the supernatant to obtain a turbid sample;
(7) freezing the turbid sample;
(8) taking out the frozen turbid sample, and freeze-drying in a vacuum freeze-drying machine at low temperature to obtain the transition metal sulfide/Ti3C2TxA composite material.
Wherein the transition metal nitrate is Co (NO)3)2·6H2O、Bi(NO3)3·5H2O、Fe(NO3)3、Mn(NO3)2·4H2One of O, Ti in step 23C2TxTi in aqueous solution3C2TxThe content of (a) is 1-2 mg/ml, and Ti in the mixed solution in the step (3)3C2TxThe mass ratio of the transition metal nitrate to the transition metal nitrate is 1: 3-7, Na in step 42Na in S aqueous solution2The content of S is 12-17 mg/ml, and Ti in the reaction mixture in the step 53C2TxWith Na2The mass ratio of S is 1: 4 to 6, Na2The S solution is added into the mixed solution within 10min after preparation, and canThe generated transition metal sulfide can be uniformly distributed in the solution, and Na is prevented2S is added too fast to cause local aggregation of transition metal sulfides, the rotating speed of a centrifuge is set to be 5000-8000 r/min in the step 6, the centrifugation time is set to be 5-10 min, the freezing time in the step 7 is 8-16 h, the freezing temperature is-15 to-25 ℃, the freezing drying temperature in a vacuum freeze dryer in the step 8 is-30 to-40 ℃, and the freeze-drying time is 12-48 h.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: 1. the resulting transition metal sulfide/Ti3C2TxThe specific surface area of the composite material is large, 3 A.g-1Specific capacitance under current density is up to 768 F.g-1(ii) a 2. Simple operation, low cost, rapidness and environmental protection.
Drawings
FIG. 1 is a SEM image of example 1;
FIG. 2 is an X-ray diffraction pattern of example 1;
FIG. 3 is a scanning electron micrograph of a comparative example;
FIG. 4 is a specific capacity curve of examples 1-3 and comparative examples at different current densities.
Detailed Description
Example 1
(1) 194mg of Bi (NO) are taken3)3·5H2Adding O into 20g of deionized water, and carrying out ultrasonic treatment for 20min to prepare Bi (NO)3)3An aqueous solution;
(2) taking 30mg of Ti3C2TxAdding into 20g deionized water, and performing ultrasonic treatment for 20min to obtain Ti3C2TxAn aqueous solution;
(3) to Bi (NO)3)3Adding Ti to the aqueous solution3C2TxStirring the aqueous solution at normal temperature for 3 hours until the aqueous solution is uniformly mixed to obtain a mixed solution;
(4) 168mg of Na2Preparing the S and 10g of deionized water into Na2S solution;
(5) mixing Na2Adding the S solution into the mixed solution in the bad step 3 within 10min, and continuing stirring for 3h until the solution is completely stirredThe reaction is complete to obtain a reaction mixture;
(6) placing the reaction mixture in a centrifuge for centrifuging for 3 times, setting the rotating speed of the centrifuge to be 5000r/min, setting the centrifuging time to be 5min, and removing supernatant liquid after the centrifugation is finished to obtain a turbid sample;
(7) freezing the turbid sample in a refrigerator at-15 ℃ for 12 h;
(8) taking out the turbid sample from the refrigerator, and freeze-drying the turbid sample in a vacuum freeze dryer at the low temperature of-40 ℃ for 12 hours to obtain Bi2S3/Ti3C2TxA composite material.
FIG. 1 shows Bi2S3/Ti3C2TxSEM image of the composite Material, from which Bi can be seen2S3/Ti3C2TxThe composite material exhibits a Ti3C2TxSupported defoliated Bi2S3Nanosheet structure, indicating a greater specific surface area and reactive centers. FIG. 2 is Bi2S3/Ti3C2TxXRD spectrum of composite material except Ti3C2TxOutside the characteristic peak of (B), Bi2S3The characteristic peak is consistent with the JCPDS card number of 65-2435, which indicates that the Bi is successfully prepared2S3/Ti3C2TxA composite material.
Adding Bi2S3/Ti3C2TxThe composite material was made into an electrode as follows: bi is weighed according to the mass ratio of 8:1:12S3/Ti3C2TxUniformly grinding the composite material, acetylene black and PTFE, uniformly dispersing the composite material by ultrasonic waves, uniformly coating the composite material on foamed nickel by using a liquid transfer gun, and drying the foamed nickel in a vacuum drying oven for 24 hours to prepare the electrode. The prepared electrode material is used as a working electrode, a saturated calomel electrode is used as a reference electrode, a platinum sheet is used as an auxiliary electrode, a 1mol/L KOH solution is used as an electrolyte solution, and an electrochemical workstation carries out cyclic voltammetry curve and constant current charge and discharge tests. The test voltage range is-1.0 to-0.2V, and the three-electrode system is utilized to testTo obtain 3 A.g-1Specific capacitance of 768F g at current density-1，Bi2S3/Ti3C2TxThe electrochemical performance of the composite material is better.
Example 2
(1) 97mg of Fe (NO) are taken3)3Adding into 20g deionized water, and performing ultrasonic treatment for 20min to obtain Fe (NO)3)3An aqueous solution;
(2) taking 30mg of Ti3C2TxAdding into 20g deionized water, and performing ultrasonic treatment for 20min to obtain Ti3C2TxAn aqueous solution;
(3) to Fe (NO)3)3Adding Ti to the aqueous solution3C2TxStirring the aqueous solution at normal temperature for 3 hours until the aqueous solution is uniformly mixed to obtain a mixed solution;
(4) 168mg of Na2Preparing the S and 10g of deionized water into Na2S solution;
(5) mixing Na2Adding the S solution into the mixed solution in the bad step 3 within 10min, and continuously stirring for 3h until the reaction is complete to obtain a reaction mixture;
(6) placing the reaction mixture in a centrifuge for centrifuging for 3 times, setting the rotating speed of the centrifuge to be 6000r/min, setting the centrifuging time to be 10min, and removing supernatant liquid after the centrifugation is finished to obtain a turbid sample;
(7) freezing the turbid sample in a refrigerator at the temperature of-25 ℃ for 8 h;
(8) taking out the turbid sample from the refrigerator, and freeze-drying at-40 deg.C for 12h in a vacuum freeze-drying machine to obtain Fe3S4-S/Ti3C2TxA composite material.
Mixing Fe3S4-S/Ti3C2TxPreparing the composite material into electrodes, assembling the electrodes into a super capacitor, and measuring 3 A.g by adopting a three-electrode system-1Specific capacitance under current density is 293.3 F.g-1。
Example 3
(1) 116mg of Co (NO) was taken3)2·6H2O is added to 2Performing ultrasonic treatment in 0g deionized water for 20min to obtain Co (NO)3)2An aqueous solution;
(2) taking 10mg of Ti3C2TxAdding into 20g deionized water, and performing ultrasonic treatment for 20min to obtain Ti3C2TxAn aqueous solution;
(3) to Co (NO)3)2Adding Ti to the aqueous solution3C2TxStirring the aqueous solution at normal temperature for 3 hours until the aqueous solution is uniformly mixed to obtain a mixed solution;
(4) 120mg of Na2Preparing the S and 10g of deionized water into Na2S solution;
(5) mixing Na2Adding the S solution into the mixed solution in the bad step 3 within 10min, and continuously stirring for 3h until the reaction is complete to obtain a reaction mixture;
(6) placing the reaction mixture in a centrifuge for centrifuging for 3 times, setting the rotating speed of the centrifuge to be 8000r/min, setting the centrifuging time to be 5min, and removing supernatant liquid after the centrifugation is finished to obtain a turbid sample;
(7) freezing the turbid sample in a refrigerator at the temperature of-20 ℃ for 16 h;
(8) taking out the turbid sample from the refrigerator, and freeze-drying the turbid sample in a vacuum freeze dryer at the low temperature of-40 ℃ for 12 hours to obtain CoS/Ti3C2TxA composite material.
Mixing CoS/Ti3C2TxPreparing the composite material into electrodes, assembling the electrodes into a super capacitor, and measuring 3 A.g by adopting a three-electrode system-1The specific capacitance under the current density is 343.3 F.g-1。
Comparative example
Taking 10mg of Ti3C2TxAdding into 20g deionized water, and carrying out ultrasonic treatment for 20min to obtain Ti3C2TxAqueous solution to Ti3C2TxAdding 20mg of deionized water into the aqueous solution, and stirring for 3 hours at normal temperature; 120mg of Na2Preparing the S and 10g of deionized water into Na2Adding the S solution into the solution within 10min, and continuously stirring for 3 h; centrifuging the aqueous solution in a centrifuge for 3 timesSetting the rotation speed of the machine to be 5000r/min, setting the centrifugation time to be 5min, and removing supernatant liquid after the centrifugation is finished to obtain a turbid sample; freezing the turbid sample in a refrigerator at-15 ℃ for 12 h; taking out the turbid sample from the refrigerator, and freeze-drying at-40 deg.C for 12h in a vacuum freeze-drying machine to obtain Ti3C2TxA material.
As can be seen from FIG. 3, Ti3C2TxThe material exhibits a distinct layered structure.
Mixing Ti3C2TxThe material is made into an electrode to assemble the super capacitor. Using a three-electrode system, 3 A.g is measured-1Specific capacitance at current density of only 77F g-1，Ti3C2TxThe electrochemical performance of the material is poor, and as can be seen from fig. 4, the transition metal sulfide/Ti obtained in example 1, example 2 and example 33C2TxThe composite material used for the electrode material can obtain higher specific capacitance value, so that the composite material is more suitable for the use of a super capacitor, and the performance of the super capacitor can be improved.
Claims (10)
1. Transition metal sulfide/Ti3C2TxThe preparation method of the composite material is characterized by comprising the following steps:
(1) adding transition metal nitrate into water to obtain transition metal nitrate water solution;
(2) mixing Ti3C2TxAdding into water to obtain Ti3C2TxAn aqueous solution;
(3) adding an aqueous solution of a transition metal nitrate to Ti3C2TxIn the water solution, uniformly stirring to obtain a mixed solution;
(4) mixing Na2Adding S into water to prepare Na2S solution;
(5) mixing Na2Adding the S solution into the mixed solution obtained in the step (3), and stirring until the reaction is complete to obtain a reaction mixture;
(6) centrifuging the reaction mixture in the step 5, and removing the supernatant to obtain a turbid sample;
(7) freezing the turbid sample;
(8) taking out the frozen turbid sample, and freeze-drying in a vacuum freeze-drying machine at low temperature to obtain the transition metal sulfide/Ti3C2TxA composite material.
2. The transition metal sulfide/Ti of claim 13C2TxThe preparation method of the composite material is characterized in that the transition metal nitrate is Co (NO)3)2·6H2O、Bi(NO3)3·5H2O、Fe(NO3)3、Mn(NO3)2·4H2And O is one of the compounds.
3. The transition metal sulfide/Ti of claim 13C2TxThe preparation method of the composite material is characterized in that Ti in the step 23C2TxTi in aqueous solution3C2TxThe content of (b) is 1-2 mg/ml.
4. The transition metal sulfide/Ti of claim 13C2TxThe preparation method of the composite material is characterized in that Ti in the mixed solution in the step 3 is added3C2TxThe mass ratio of the transition metal nitrate to the transition metal nitrate is 1: 3 to 7.
5. The transition metal sulfide/Ti of claim 13C2TxThe preparation method of the composite material is characterized in that Na is adopted in the step 42Na in S aqueous solution2The content of S is 12-17 mg/ml.
6. The transition metal sulfide/Ti of claim 13C2TxThe preparation method of the composite material is characterized in that Ti in the reaction mixture in the step 53C2TxWith Na2The mass ratio of S is 1: 4 to 6.
7. The transition metal sulfide/Ti of claim 13C2TxThe preparation method of the composite material is characterized in that Na in the step 52And adding the S solution into the mixed solution within 10min after preparation.
8. The transition metal sulfide/Ti of claim 13C2TxThe preparation method of the composite material is characterized in that the rotating speed of a centrifugal machine in the step 6 is set to be 5000-8000 r/min, and the centrifugal time is set to be 5-10 min.
9. The transition metal sulfide/Ti of claim 13C2TxThe preparation method of the composite material is characterized in that the freezing time in the step 7 is 8-16 h, and the freezing temperature is-15 to-25 ℃.
10. The transition metal sulfide/Ti of claim 13C2TxThe preparation method of the composite material is characterized in that in the step 8, the freeze drying temperature in the vacuum freeze dryer is-30 to-40 ℃, and the freeze drying time is 12 to 48 hours.
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| CN114527175A (en) * | 2022-02-14 | 2022-05-24 | 常州大学 | Self-powered photovoltaic adapter sensor based on sulfur vacancy as well as preparation method and application thereof |
| CN114849748A (en) * | 2022-05-13 | 2022-08-05 | 华东理工大学 | CoS/Ti 3 C 2 Preparation and application of MXene composite material |
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