CN107230560A - A kind of method that microwave radiation prepares titanium dioxide/stratiform carbon composite - Google Patents
A kind of method that microwave radiation prepares titanium dioxide/stratiform carbon composite Download PDFInfo
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- CN107230560A CN107230560A CN201710566349.5A CN201710566349A CN107230560A CN 107230560 A CN107230560 A CN 107230560A CN 201710566349 A CN201710566349 A CN 201710566349A CN 107230560 A CN107230560 A CN 107230560A
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- titanium dioxide
- carbon composite
- stratiform carbon
- microwave
- stratiform
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 47
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 46
- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 25
- 230000005855 radiation Effects 0.000 title claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910009819 Ti3C2 Inorganic materials 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005530 etching Methods 0.000 claims abstract description 9
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 6
- 238000000967 suction filtration Methods 0.000 claims abstract description 6
- 239000010936 titanium Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 238000000151 deposition Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims 1
- 229910052731 fluorine Inorganic materials 0.000 claims 1
- 239000011737 fluorine Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 13
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 239000007772 electrode material Substances 0.000 description 8
- -1 conductive black Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 239000006260 foam Substances 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000003610 charcoal Substances 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 238000004513 sizing Methods 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 241000446313 Lamella Species 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 241000872198 Serjania polyphylla Species 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000004087 circulation Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000011267 electrode slurry Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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 OR LIGHT-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 OR LIGHT-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 OR LIGHT-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
- H01G11/46—Metal oxides
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
It is by ternary MAX phase materials Ti the invention discloses a kind of preparation method of titanium dioxide/stratiform carbon composite3AlC2Powder is soaked ternary MAX phase materials Ti3AlC2Powder is soaked in a solution of hydrofluoric acid, and reaction is performed etching under continuous stirring；Reaction terminates rear suction filtration, and product is cleaned repeatedly with distilled water and absolute ethyl alcohol, obtains black powder product, dries, obtains depositing apertured Ti between synusia3C2TxStratified material；Again by Ti3C2TxWith conductive black mixed grinding it is uniform after, be put into microwave heating equipment, titanium dioxide/stratiform carbon composite obtained after microwave radiation.The method of titanium dioxide prepared by the present invention/stratiform carbon composite is simple, and reaction condition is gentle, and energy consumption is low；Preparation time is shorter, efficiency high.The titanium dioxide of acquisition/stratiform carbon composite has excellent chemical property, applies on ultracapacitor, possesses higher specific capacitance and excellent cyclical stability.
Description
Technical field
The present invention relates to a kind of preparation method of titanium dioxide/stratiform carbon composite, more particularly to a kind of microwave radiation
The method for preparing titanium dioxide/stratiform carbon composite, is mainly used as the electrode material of ultracapacitor.
Background technology
With developing rapidly for World Economics, energy crisis and problem of environmental pollution are very important, and development one kind can
The energy and energy storage mode of lasting clean and effective are extremely urgent.Ultracapacitor is used as a kind of efficient, cleaning, sustainable energy
Source device, is received significant attention.Ultracapacitor has good power density high and low temperature performance, service life length and high security
The advantages of, electronic product and energy regenerating and field of storage can be widely applied to.
Two-dimensional layer titanium carbide, it is excellent due to its unique appearance structure, less particle size, larger specific surface area
Different electric conductivity, big specific surface area and high magnification stability and with superpower chemical property, be widely used in electric capacity
In device, lithium ion battery, solar cell etc..Nano titanium oxide not only have fabulous high rate capability, cyclical stability,
Fast charging and discharging performance and higher capacity, nano titanium oxide can also effectively reduce the capacity attenuation of capacitor, increase electric capacity
Device stability, improves chemical property.Titanium dioxide/stratiform carbon composite combines two-dimensional layer carbon and nano titanium oxide
Characteristic, with good electric conductivity, chemical stability, heat endurance, nontoxicity etc., be widely used in capacitor, lithium from
In sub- battery etc..
The method for preparing titanium dioxide/stratiform carbon material at present uses hydro-thermal method and in-situ method mostly, and hydro-thermal method needs height
Temperature is reacted, and high energy consumption, cost is also high；In-situ method needs the longer reaction time, and efficiency is low；And mainly as lithium ion
The electrode material of battery, sodium-ion battery.
The content of the invention
The purpose of the present invention is to be directed to hydro-thermal method and in-situ method high energy consumption, and there is provided a kind of microwave radiation for the problem of efficiency is low
The method of synthesis of titanium dioxide/stratiform carbon composite；
First, the preparation of titanium dioxide/stratiform carbon composite
The method that microwave radiation of the present invention prepares titanium dioxide/stratiform carbon composite, is comprised the following steps that：
（1）Ti3C2TxThe preparation of stratified material：By ternary MAX phase materials Ti3AlC2Powder（Granularity is 500 ~ 2000 mesh）Immersion
In 10 ~ 40 wt% hydrofluoric acid solutions, under continuous stirring in 20 ~ 50 °C of 2 ~ 24h of etching reaction；Reaction terminates rear suction filtration, produces
Thing is cleaned repeatedly with distilled water and absolute ethyl alcohol, is obtained black powder product, is placed in drying box, in 40 ~ 80 °C of lower heat preservation and drynesses 8
~ 24 h, obtain depositing apertured Ti between synusia3C2TxStratified material；
（2）The preparation of titanium dioxide/stratiform carbon composite：By Ti3C2TxWith conductive black with 1:0.01~1:0.1 mass ratio
It is fully ground, is then placed in microwave heating equipment after mixing, in the case where power is 600 ~ 1200 W, the s of microwave radiation 10 ~ 60 is obtained
To titanium dioxide/stratiform carbon composite.
Fig. 1（a）For the Ti after hf etching3AlC2Powder（Ti3C2TxStratified material）SEM figure, Fig. 1（b）For
The SEM figures of titanium dioxide/stratiform carbon composite.By Fig. 1（b）And illustration can be seen that stratiform carbon material Ti3C2TxLamella
Structure is substantially thinning, and the more uniform titanium dioxide granule of size is all generated in surface and lamellar structure, is grown in piece
Obvious two lamellas of connection of nano particle in layer, which forms a more coarse three-dimensional structure, this structure is favourable
In titanium dioxide/application of the stratiform carbon composite on ultracapacitor.
2nd, the chemical property of titanium dioxide/stratiform carbon composite
It is 8 by mass ratio to test the chemical property of titanium dioxide/stratiform carbon composite:1:1 titanium dioxide/stratiform
Carbon nano-composite material, conductive black, polytetrafluoroethylene (PTFE)（PTFE）Electrode slurry is mixed into, slurry then is dispersed in into area is
1 cm2In foam nickel sheet, electrode is then dried into 8 ~ 24 h under 40 ~ 80 °C, titanium dioxide/stratiform carbon electricity has been finally given
Pole.Electrode carries out electrochemical property test to it under three-electrode system using 3 mol/LKOH electrolyte, reference electrode and right
Electrode is Hg/HgO and platinum plate electrode respectively.Electrode material is entered under 1 A/g current density respectively using electrochemical workstation
Row constant current charge-discharge tests the specific capacitance for obtaining electrode material, is passed through using battery test system under 1 A/g current density
5000 circulations are crossed, its cyclical stability is investigated.Shown by the test result of chemical property, the electrode material is in 1 A/g
Current density under specific capacitance up to 171 F/g, circulated by 5000 constant current charge-discharges, specific capacitance for 91 original % with
On.
In summary, microwave radiation of the present invention prepare titanium dioxide/stratiform carbon composite method it is simple, reaction condition
Gently, energy consumption is low；Preparation time is shorter, efficiency high.The titanium dioxide of acquisition/stratiform carbon composite has excellent electrochemistry
Performance, is applied on ultracapacitor, with higher specific capacitance and excellent cyclical stability.
Brief description of the drawings
Fig. 1 is the Ti after over etching3AlC2Powder（a）And titanium dioxide/stratiform carbon composite（b）SEM figure.
Embodiment
It is following to pass through specific preparation method and performance of the specific embodiment to titanium dioxide of the present invention/stratiform carbon composite
It is described further.
Embodiment 1
（1）Ti3C2TxThe preparation of stratified material：By 0.1946 g ternary MAX phase materials Ti3AlC2Powder（Granularity is 500 ~ 2000
Mesh）It is immersed in the wt% hydrofluoric acid solutions of 30 mL 20, continuing magnetic force is stirred in 20 DEG C of h of etching reaction 24, course of reaction；
Suction filtration afterwards, product distilled water and each three times of washes of absolute alcohol, obtain black powder product, place into drying box in 50
DEG C dry 18 h, produce Ti3C2TxStratified material；
（2）The preparation of titanium dioxide/stratiform carbon composite：Take Ti3C2TxThe mg of stratified material 200, the mg of conductive black 20, puts
Enter in agate mortar, 30 min are to uniform for grinding, be then placed in microwave reaction device, 60 are radiated under the W of microwave power 600
S, that is, obtain titanium dioxide/stratiform carbon composite.
（3）The chemical property of titanium dioxide/stratiform carbon composite：Take titanium dioxide/mg of stratiform carbon 40, conductive charcoal
Black 5 mg and polytetrafluoroethylene (PTFE) 5 mg, is mixed into after uniform sizing material by ethanol and is dispersed in area for 1 cm2In foam nickel sheet, 60
12 h are dried at DEG C.By the test of chemical property, electrode material specific capacitance under 1 A/g current density is 171 F/g,
Circulated by 5000 constant current charge-discharges, specific capacitance is original 93%.Therefore, with higher specific capacitance and excellent follow
Ring stability.
Embodiment 2
（1）Ti3C2TxThe preparation of stratified material：By 0.5 g ternary MAX phase materials Ti3AlC2Powder（Granularity is 500 ~ 2000 mesh）
It is immersed in the wt% hydrofluoric acid solutions of 50 mL 30, continuing magnetic force is stirred in 40 DEG C of h of etching reaction 12, course of reaction；Afterwards
Suction filtration, product distilled water and each three times of washes of absolute alcohol, obtain black powder product, place into drying box dry in 60 DEG C
Dry 24 h, produces Ti3C2TxStratified material；
（2）The preparation of titanium dioxide/stratiform carbon composite：Take Ti3C2TxThe mg of the stratified material 100 and mg of conductive black 1, puts
Enter in agate mortar, 10 min are to uniform for grinding, are then placed in microwave reaction device, radiated in the case where microwave power is 700 W
10 s, that is, obtain titanium dioxide/stratiform carbon composite.
（3）The chemical property of titanium dioxide/stratiform carbon composite：Take titanium dioxide/mg of stratiform carbon 80, conductive charcoal
Black 10 mg and polytetrafluoroethylene (PTFE) 10 mg, is mixed into after uniform sizing material by ethanol and is dispersed in area for 1 cm2In foam nickel sheet,
24 h are dried at 40 DEG C.By the test of chemical property, electrode material specific capacitance under 1 A/g current density is 162
F/g, is circulated by 5000 constant current charge-discharges, and specific capacitance is original 92%.Therefore, with higher specific capacitance and excellent
Cyclical stability.
Embodiment 3
（1）Ti3C2TxThe preparation of stratified material
By 0.937 g ternary MAX phase materials Ti3AlC2Powder（Granularity is 500 ~ 2000 mesh）It is immersed in 40 mL, 40 wt% hydrogen
In fluorspar acid solution, continuing magnetic force is stirred in 50 DEG C of h of etching reaction 18, course of reaction；Suction filtration afterwards, product distilled water and
Each three times of washes of absolute alcohol, obtains black powder product, places into drying box in 40 DEG C of dry 12 h, produces Ti3C2TxLayer
Shape material；
（2）The preparation of titanium dioxide/stratiform carbon composite：Take Ti3C2TxThe mg of the stratified material 200 and mg of conductive black 4, puts
Enter in agate mortar, 20 min are to uniform for grinding, be then placed in microwave reaction device, 30 are radiated under the W of microwave power 800
S, that is, obtain titanium dioxide/stratiform carbon composite.
（3）The chemical property of titanium dioxide/stratiform carbon composite：Take titanium dioxide/mg of stratiform carbon 48, conductive charcoal
Black 6 mg and polytetrafluoroethylene (PTFE) 6 mg, is mixed into after uniform sizing material by ethanol and is dispersed in area for 1 cm2In foam nickel sheet, 70
10 h are dried at DEG C.By the test of chemical property, electrode material specific capacitance under 1 A/g current density is 157 F/g,
Circulated by 5000 constant current charge-discharges, specific capacitance is original 91%.Therefore, with higher specific capacitance and excellent follow
Ring stability.
Claims (7)
1. a kind of method that microwave method prepares titanium dioxide/stratiform carbon composite, comprises the following steps：
（1）Ti3C2TxThe preparation of stratified material：By ternary MAX phase materials Ti3AlC2Powder soaks in a solution of hydrofluoric acid, is holding
Reaction is performed etching under continuous stirring；Reaction terminates rear suction filtration, and product is cleaned repeatedly with distilled water and absolute ethyl alcohol, obtains black powder
Last product, dries, obtains depositing apertured Ti between synusia3C2TxStratified material；
（2）The preparation of titanium dioxide/stratiform carbon composite：By Ti3C2TxWith conductive black mixed grinding it is uniform after, be put into micro-
Titanium dioxide/stratiform carbon composite is obtained in Wave heating device, after microwave radiation.
2. the method that microwave method as claimed in claim 1 prepares titanium dioxide/stratiform carbon composite, it is characterised in that：Ternary
MAX phase materials Ti3AlC2Powder size is 500 ~ 2000 mesh.
3. the method that microwave method as claimed in claim 1 prepares titanium dioxide/stratiform carbon composite, it is characterised in that：Hydrogen fluorine
Acid concentration is 10 ~ 40 wt%.
4. the method that microwave method as claimed in claim 3 prepares titanium dioxide/stratiform carbon composite, it is characterised in that：Ternary
MAX phase materials Ti3AlC2Time in powder immersion hydrofluoric acid is 2 ~ 24h, and its etching temperature is 20 ~ 50 °C.
5. the method that microwave method as claimed in claim 1 prepares titanium dioxide/stratiform carbon composite, it is characterised in that：It is described
Ti3C2TxStratified material is dried, and is that 8 ~ 24 h are dried under 40 ~ 80 °C.
6. the method that microwave method as claimed in claim 1 prepares titanium dioxide/stratiform carbon composite, it is characterised in that：It is described
Conductive black and Ti3C2TxThe mass ratio of stratified material is 1:0.01~1:0.1.
7. the method that microwave method as claimed in claim 1 prepares titanium dioxide/stratiform carbon composite, it is characterised in that：Microwave
The power of radiation is 600 ~ 1200 W, and microwave irradiation time is 10 ~ 60 s.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108461300A (en) * | 2018-05-11 | 2018-08-28 | 西北师范大学 | A kind of stratiform titanium carbide-carbon pipe composite material and its preparation and application |
| CN109647464A (en) * | 2019-01-09 | 2019-04-19 | 青岛大学 | A kind of electrocatalysis material converting nitrogen to ammonia |
| CN110098391A (en) * | 2019-04-18 | 2019-08-06 | 北京化工大学 | Titanium dioxide/carbon-coated nano silicon trielement composite material derived from a kind of MXene and preparation method thereof |
| CN110817875A (en) * | 2019-12-20 | 2020-02-21 | 武汉科技大学 | Ti3AlC2Powder and preparation method thereof |
| CN111151276A (en) * | 2020-01-19 | 2020-05-15 | 中南大学 | Full-spectrum photocatalytic synthesis of ammonia Ti3C2Tx/TiO2Composite material and preparation method and application thereof |
| TWI711584B (en) * | 2018-12-28 | 2020-12-01 | 日商亞都瑪科技股份有限公司 | MXene particle material, slurry, secondary battery, transparent electrode, manufacturing method of MXene particle material |
| CN112599762A (en) * | 2020-12-15 | 2021-04-02 | 南京国轩电池有限公司 | TiO 22Negative electrode material of CNF battery and preparation method thereof |
| CN113410454A (en) * | 2021-06-09 | 2021-09-17 | 昆明理工大学 | Preparation method and application of porous layered titanium dioxide |
| CN113690066A (en) * | 2021-08-10 | 2021-11-23 | 太原理工大学 | Graphene quantum dot/few-layer Ti3C2TxPreparation method and application of composite material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104496461A (en) * | 2014-12-23 | 2015-04-08 | 陕西科技大学 | Method for preparing cubic titanium dioxide/two-dimensional nano-titanium carbide composite material |
| CN105084360A (en) * | 2015-09-14 | 2015-11-25 | 哈尔滨工业大学 | Method for stripping two-dimensional nano Ti3C2 lamella by adopting microwave heating assisted ultrasonic method |
-
2017
- 2017-07-12 CN CN201710566349.5A patent/CN107230560B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104496461A (en) * | 2014-12-23 | 2015-04-08 | 陕西科技大学 | Method for preparing cubic titanium dioxide/two-dimensional nano-titanium carbide composite material |
| CN105084360A (en) * | 2015-09-14 | 2015-11-25 | 哈尔滨工业大学 | Method for stripping two-dimensional nano Ti3C2 lamella by adopting microwave heating assisted ultrasonic method |
Non-Patent Citations (2)
| Title |
|---|
| MEIKANG HAN等: "Laminated and Two-Dimensional Carbon-Supported Microwave Absorbers Derived from MXenes", 《APPL. MATER. INTERFACES》 * |
| XINLIANG LI等: "A controllable heterogeneous structure and electromagnetic wave absorption properties of Ti2CTx MXene", 《JOURNAL OF MATERIALS CHEMISTRY C》 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108461300A (en) * | 2018-05-11 | 2018-08-28 | 西北师范大学 | A kind of stratiform titanium carbide-carbon pipe composite material and its preparation and application |
| CN108461300B (en) * | 2018-05-11 | 2020-05-12 | 西北师范大学 | Layered titanium carbide-carbon tube composite material and preparation and application thereof |
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