CN109402662A - A kind of preparation method of selenizing molybdenum two-dimensional layer carbonization titanium composite material - Google Patents
A kind of preparation method of selenizing molybdenum two-dimensional layer carbonization titanium composite material Download PDFInfo
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- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
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- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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- C—CHEMISTRY; METALLURGY
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- 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
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- 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
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
A kind of preparation method of selenizing molybdenum two-dimensional layer carbonization titanium composite material, it is related to a kind of preparation of metal carbides/sulfide composite material.The invention solves the electric conductivity of existing selenizing molybdenum is poor, the lower problem of ionic mobility.Method: one, Se powder and hydrazine hydrate are mixed, obtain selenium-hydrazine hydrate dispersion liquid；MXene-Ti3C2Dispersion liquid is mixed with cetyl trimethylammonium bromide, and sodium molybdate is added, obtains cetyl trimethylammonium bromide solution；Three, by selenium-hydrazine hydrate dispersion liquid and cetyl trimethylammonium bromide solution hybrid reaction, mixed solution is obtained；Four, mixed solution deionized water and ethyl alcohol are cleaned and is centrifuged, vacuum drying obtains MoSe2@MXene‑Ti3C2Composite material.Preparation of the present invention for selenizing molybdenum two-dimensional layer carbonization titanium composite material.
Description
Technical field
The present invention relates to a kind of preparations of metal carbides/sulfide composite material.
Background technique
Two-dimentional transition metal carbides (Mxene) have unique layer structure, excellent electric conductivity, electro-chemical activity
High, large specific surface area, has great application potential in electro-catalysis and energy storage field.
Selenizing molybdenum is combined by weaker Van der Waals force between layers as one of magnesium-yttrium-transition metal chalcogenide, because
This can be stripped into two-dimentional class graphene-structured, to obtain the unique electronic property different from body material.The exposure of its edge
Active site make it have electro catalytic activity.And its interlamellar spacing is larger, some ions can be readily intercalated into selenizing molybdenum lamella it
Between, therefore also there is good energy storage effect.But its intrinsic conductivity is poor, and ionic mobility is lower, leads to high rate performance not
It is good, it is limited in the application of energy storage field；Same because electric conductivity is poor, reaction barrier increases, and the prior art passes through to selenium
Change molybdenum and carry out defect regulation, liberation of hydrogen is that current density is 10mA/cm2When, overpotential 305mV, thus limit its
The application of catalysis and energy storage field.
Summary of the invention
The invention solves the electric conductivity of existing selenizing molybdenum is poor, the lower problem of ionic mobility, and a kind of selenium is provided
Change the preparation method of molybdenum two-dimensional layer carbonization titanium composite material.
A kind of preparation method of selenizing molybdenum two-dimensional layer carbonization titanium composite material carries out according to the following steps:
One, 12h~for 24 hours is mixed in the hydrazine hydrate that Se powder and mass percent are 97%~98%, obtains selenium-hydration
The dispersion liquid of hydrazine；
The volume ratio of mole hydrazine hydrate for being 97%~98% with mass percent of the Se powder is (0.8~1.3)
mmol:5mL；
Two, by MXene-Ti3C2Dispersion liquid is mixed with cetyl trimethylammonium bromide, is 30 DEG C~50 DEG C in temperature
Under the conditions of, 0.5h~2h is stirred, sodium molybdate is added and stirs 0.2h~2h, obtains cetyl trimethylammonium bromide solution；
The MXene-Ti3C2The volume of dispersion liquid and the mass ratio of cetyl trimethylammonium bromide are (10~50)
mL:1g；The MXene-Ti3C2The volume of dispersion liquid and the molar ratio of sodium molybdate are (10~15) mL:1mmol；
The MXene-Ti3C2Dispersion liquid carries out according to the following steps: being 8.5mol/L 1., by lithium fluoride and concentration
The mixed in hydrochloric acid of~9.5mol/L simultaneously stirs 25min~35min, obtains mixed solution A；
The volume ratio for the hydrochloric acid that the quality of the lithium fluoride and concentration are 8.5mol/L~9.5mol/L be 1g:(30~
50)mL；
2., with the speed of 1mL/s~3mL/s, by MAX-Ti3AlC2Be added in mixed solution A, temperature be 35 DEG C~
Under conditions of 45 DEG C, stirring 20h~for 24 hours, obtain reaction solution；
The MAX-Ti3AlC2Quality and mixed solution A volume ratio be 1g:(10~20) mL；
3., revolving speed be 3000rpm~4000rpm under conditions of, by reaction solution be centrifuged 8min~12min, gone after centrifugation
Fall supernatant, obtains sediment；
4., deionized water is added into sediment, be uniformly mixed, obtain precipitated liquid, ultrasonic power be 700W~800W
Under conditions of, then precipitated liquid ultrasound 10min~20min is centrifuged under conditions of revolving speed is 3000rpm~4000rpm
5min~15min removes supernatant, the sediment after obtaining once washing；
The quality of the sediment and the volume ratio of deionized water are 1g:(30~40) mL；
5., 4. the sediment after once washing repeated by step, until supernatant pH is 4~5, sinking after wash
Starch；
6., into the sediment after washing ethyl alcohol is added, obtain mixed solution B, be 700W~800W's in ultrasonic power
Under the conditions of, to mixed solution B ultrasound sound 0.8h~1.2h, then it is centrifuged under conditions of revolving speed is 8000rpm~10000rpm
10min~15min, the lower sediment thing after obtaining ethyl alcohol cleaning；
The percentage by volume of sediment after washing in the mixed solution B is 5%~10%；
7., into the lower sediment thing after ethyl alcohol cleaning deionized water is added, be uniformly mixed, obtain mixed solution C, super
Acoustical power be 700W~800W under conditions of, to mixed solution C ultrasound 20min~30min, then revolving speed be 3000rpm~
It is centrifuged 2min~4min under conditions of 4000rpm, takes black rice-pudding color upper liquid dry, obtains MXene-Ti3C2, by MXene-Ti3C2With
Water mixing, obtains MXene-Ti3C2Dispersion liquid；The MXene-Ti3C2Dispersion liquid concentration is 10mg/mL~15mg/mL；
The percentage by volume of lower sediment thing in the mixed solution C after ethyl alcohol cleaning is 2%~2.5%；
Three, selenium-hydrazine hydrate dispersion liquid and cetyl trimethylammonium bromide solution are mixed into simultaneously magnetic agitation, then existed
Under conditions of reaction temperature is 160 DEG C~200 DEG C, 8h~16h is reacted, mixed solution D is obtained；
The volume ratio of selenium-hydrazine hydrate dispersion liquid and cetyl trimethylammonium bromide solution be (1.6~
2.2):1；
Four, mixed solution D deionized water and ethyl alcohol are cleaned and is centrifuged, the condition for being finally 30 DEG C~50 DEG C in temperature
Under, vacuum drying 1h~5h obtains MoSe2@MXene-Ti3C2Composite material completes a kind of selenizing molybdenum two-dimensional layer titanium carbide
The preparation method of composite material.
The beneficial effects of the present invention are:
MoSe prepared by the present invention2@MXene-Ti3C2Composite material has the performance of good electro-catalysis hydrolytic hydrogen production, electricity
Current density is 10mA/cm2When, MoSe2Overpotential is 360mV, and MoSe2@MXene-Ti3C2Overpotential be 260mV, MXene
Addition be substantially reduced the overpotential of evolving hydrogen reaction, this is because improving the intrinsic conductivity of material by MXene phase, make
Electronics can be transmitted largely during reaction, and the composite material being prepared into is spherical micro nano structure, and large specific surface area is living
Property site it is more, load capacity is high, so as to effectively improve catalytic performance.
MoSe prepared by the present invention2@MXene-Ti3C2There is composite material good lithium (sodium) battery performance to be,
MXene-Ti3C2High conductivity, unique micro-sphere structure shortens Ion transfer path, improves ionic mobility, thus
Improve high rate performance.
The present invention utilizes hydro-thermal method one-step synthesis MXene-Ti3C2/MoSe2Composite material, preparation method are simple, at low cost
It is honest and clean, be easy to regulate and control, be convenient for industrialized production, have a wide range of applications in the fields such as water electrolysis hydrogen production and energy storage electrode.
Detailed description of the invention
Fig. 1 is MoSe prepared by embodiment one2@MXene-Ti3C2The transmission electron microscopy figure of composite material；
Fig. 2 is MoSe2@MXene-Ti3C2And MoSe2Linear scan curve graph, 1 is MoSe2, 2 prepare for embodiment one
MoSe2@MXene-Ti3C2Composite material.
Specific embodiment
Specific embodiment 1: a kind of preparation method of selenizing molybdenum two-dimensional layer carbonization titanium composite material of present embodiment is
It carries out according to the following steps:
One, 12h~for 24 hours is mixed in the hydrazine hydrate that Se powder and mass percent are 97%~98%, obtains selenium-hydration
The dispersion liquid of hydrazine；
The volume ratio of mole hydrazine hydrate for being 97%~98% with mass percent of the Se powder is (0.8~1.3)
mmol:5mL；
Two, by MXene-Ti3C2Dispersion liquid is mixed with cetyl trimethylammonium bromide, is 30 DEG C~50 DEG C in temperature
Under the conditions of, 0.5h~2h is stirred, sodium molybdate is added and stirs 0.2h~2h, obtains cetyl trimethylammonium bromide solution；
The MXene-Ti3C2The volume of dispersion liquid and the mass ratio of cetyl trimethylammonium bromide are (10~50)
mL:1g；The MXene-Ti3C2The volume of dispersion liquid and the molar ratio of sodium molybdate are (10~15) mL:1mmol；
The MXene-Ti3C2Dispersion liquid carries out according to the following steps: being 8.5mol/L 1., by lithium fluoride and concentration
The mixed in hydrochloric acid of~9.5mol/L simultaneously stirs 25min~35min, obtains mixed solution A；
The volume ratio for the hydrochloric acid that the quality of the lithium fluoride and concentration are 8.5mol/L~9.5mol/L be 1g:(30~
50)mL；
2., with the speed of 1mL/s~3mL/s, by MAX-Ti3AlC2Be added in mixed solution A, temperature be 35 DEG C~
Under conditions of 45 DEG C, stirring 20h~for 24 hours, obtain reaction solution；
The MAX-Ti3AlC2Quality and mixed solution A volume ratio be 1g:(10~20) mL；
3., revolving speed be 3000rpm~4000rpm under conditions of, by reaction solution be centrifuged 8min~12min, gone after centrifugation
Fall supernatant, obtains sediment；
4., deionized water is added into sediment, be uniformly mixed, obtain precipitated liquid, ultrasonic power be 700W~800W
Under conditions of, then precipitated liquid ultrasound 10min~20min is centrifuged under conditions of revolving speed is 3000rpm~4000rpm
5min~15min removes supernatant, the sediment after obtaining once washing；
The quality of the sediment and the volume ratio of deionized water are 1g:(30~40) mL；
5., 4. the sediment after once washing repeated by step, until supernatant pH is 4~5, sinking after wash
Starch；
6., into the sediment after washing ethyl alcohol is added, obtain mixed solution B, be 700W~800W's in ultrasonic power
Under the conditions of, to mixed solution B ultrasound sound 0.8h~1.2h, then it is centrifuged under conditions of revolving speed is 8000rpm~10000rpm
10min~15min, the lower sediment thing after obtaining ethyl alcohol cleaning；
The percentage by volume of sediment after washing in the mixed solution B is 5%~10%；
7., into the lower sediment thing after ethyl alcohol cleaning deionized water is added, be uniformly mixed, obtain mixed solution C, super
Acoustical power be 700W~800W under conditions of, to mixed solution C ultrasound 20min~30min, then revolving speed be 3000rpm~
It is centrifuged 2min~4min under conditions of 4000rpm, takes black rice-pudding color upper liquid dry, obtains MXene-Ti3C2, by MXene-Ti3C2With
Water mixing, obtains MXene-Ti3C2Dispersion liquid；The MXene-Ti3C2Dispersion liquid concentration is 10mg/mL~15mg/mL；
The percentage by volume of lower sediment thing in the mixed solution C after ethyl alcohol cleaning is 2%~2.5%；
Three, selenium-hydrazine hydrate dispersion liquid and cetyl trimethylammonium bromide solution are mixed into simultaneously magnetic agitation, then existed
Under conditions of reaction temperature is 160 DEG C~200 DEG C, 8h~16h is reacted, mixed solution D is obtained；
The volume ratio of selenium-hydrazine hydrate dispersion liquid and cetyl trimethylammonium bromide solution be (1.6~
2.2):1；
Four, mixed solution D deionized water and ethyl alcohol are cleaned and is centrifuged, the condition for being finally 30 DEG C~50 DEG C in temperature
Under, vacuum drying 1h~5h obtains MoSe2@MXene-Ti3C2Composite material completes a kind of selenizing molybdenum two-dimensional layer titanium carbide
The preparation method of composite material.
The beneficial effect of present embodiment is:
The MoSe of present embodiment preparation2@MXene-Ti3C2Composite material has good electro-catalysis hydrolytic hydrogen production
Performance, current density 10mA/cm2When, MoSe2Overpotential is 360mV, and MoSe2@MXene-Ti3C2Overpotential be
The addition of 260mV, MXene are substantially reduced the overpotential of evolving hydrogen reaction, this is because improving the sheet of material by MXene phase
Conductivity to be levied, transmits electronics during reaction largely, the composite material being prepared into is spherical micro nano structure, than
Surface area is big, and active site is more, and load capacity is high, so as to effectively improve catalytic performance.
The MoSe of present embodiment preparation2@MXene-Ti3C2Composite material has good lithium (sodium) battery performance
It is, MXene-Ti3C2High conductivity, unique micro-sphere structure shortens Ion transfer path, improves ionic mobility,
To improve high rate performance.
Present embodiment utilizes hydro-thermal method one-step synthesis MXene-Ti3C2/MoSe2Composite material, preparation method letter
It is single, low in cost, be easy to regulate and control, be convenient for industrialized production, have in the fields such as water electrolysis hydrogen production and energy storage electrode extensive
Application prospect.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: Se powder described in step 1
Mole hydrazine hydrate for being 97%~98% with mass percent volume ratio be (0.8~1) mmol:5mL.Other and specific reality
It is identical to apply mode one.
Specific embodiment 3: unlike one of present embodiment and specific embodiment one or two: institute in step 2
The MXene-Ti stated3C2The volume of dispersion liquid and the mass ratio of cetyl trimethylammonium bromide are (10~40) mL:1g；Step
MXene-Ti described in two3C2The volume of dispersion liquid and the molar ratio of sodium molybdate are (10~12) mL:1mmol.It is other with it is specific
Embodiment one or two is identical.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: will in step 2
MXene-Ti3C2Dispersion liquid is mixed with cetyl trimethylammonium bromide, under conditions of temperature is 30 DEG C~45 DEG C, stirs 1h
~2h is added sodium molybdate and stirs 1h~2h, obtains cetyl trimethylammonium bromide solution.It is other with specific embodiment one to
Three is identical.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four: step 2 1. in
It is the mixed in hydrochloric acid of 8.5mol/L~9mol/L by lithium fluoride and concentration and stirs 25min~30min, obtains mixed solution A；Institute
The volume ratio for the hydrochloric acid that the quality and concentration for the lithium fluoride stated are 8.5mol/L~9mol/L is 1g:(30~40) mL.It is other with
Specific embodiment one is to four identical.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: step 2 2. in
With the speed of 1mL/s~2mL/s, by MAX-Ti3AlC2It is added in mixed solution A, the condition for being 35 DEG C~40 DEG C in temperature
Under, stirring 22h~for 24 hours, obtain reaction solution；The MAX-Ti3AlC2Quality and mixed solution A volume ratio be 1g:(15
~20) mL.It is other identical as specific embodiment one to five.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: step 2 4. in
Deionized water is added into sediment, is uniformly mixed, obtains precipitated liquid, it, will under conditions of ultrasonic power is 750W~800W
Then precipitated liquid ultrasound 15min~20min is centrifuged 5min~10min under conditions of revolving speed is 3500rpm~4000rpm, goes
Fall supernatant, the sediment after obtaining once washing；The quality of the sediment and the volume ratio of deionized water are 1g:(35
~40) mL.It is other identical as specific embodiment one to six.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven: step 2 6. in
Ethyl alcohol is added into the sediment after washing, obtains mixed solution B, under conditions of ultrasonic power is 750W~800W, to mixed
Solution B ultrasound 1h~1.2h is closed, 12min~15min is then centrifuged under conditions of revolving speed is 9000rpm~10000rpm, is obtained
Lower sediment thing to after ethyl alcohol cleaning；In the mixed solution B wash after sediment percentage by volume be 5%~
8%.It is other identical as specific embodiment one to seven.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight: step 2 7. in
Deionized water is added into the lower sediment thing after ethyl alcohol cleaning, is uniformly mixed, obtains mixed solution C, be in ultrasonic power
It is then 3500rpm~4000rpm's in revolving speed to mixed solution C ultrasound 25min~30min under conditions of 750W~800W
Under the conditions of be centrifuged 2min~3min, take black rice-pudding color upper liquid dry, obtain MXene-Ti3C2, by MXene-Ti3C2It mixes, obtains with water
To MXene-Ti3C2Dispersion liquid；The MXene-Ti3C2Dispersion liquid concentration is 10mg/mL~14mg/mL.Other and specific reality
It is identical to apply mode one to eight.
Specific embodiment 10: unlike one of present embodiment and specific embodiment one to nine: step 3 is by selenium-
The dispersion liquid and cetyl trimethylammonium bromide solution of hydrazine hydrate mix and magnetic agitation, is then 180 DEG C in reaction temperature
Under conditions of~200 DEG C, 8h~12h is reacted, mixed solution D is obtained；Selenium-hydrazine hydrate dispersion liquid and cetyl three
The volume ratio of methyl bromide ammonium salt solution is (1.6~2): 1.It is other identical as specific embodiment one to nine.
Beneficial effects of the present invention are verified using following embodiment:
Embodiment one:
A kind of preparation method of selenizing molybdenum two-dimensional layer carbonization titanium composite material carries out according to the following steps:
One, 20h is mixed in the hydrazine hydrate that 2mmol Se powder and 10mL mass percent are 98%, obtains selenium-hydration
The dispersion liquid of hydrazine；
Two, by 10mL MXene-Ti3C2Dispersion liquid is mixed with 0.33g cetyl trimethylammonium bromide, is 45 in temperature
Under conditions of DEG C, 1h is stirred, 1mmol sodium molybdate is added and stirs 1h, obtains cetyl trimethylammonium bromide solution；
The MXene-Ti3C2Dispersion liquid carries out according to the following steps: 1., by 1g lithium fluoride and 40mL concentration being
The mixed in hydrochloric acid of 9mol/L simultaneously stirs 30min, obtains mixed solution A；
2., with 1mL/s speed, by 2g MAX-Ti3AlC2It is added in 40mL mixed solution A, the item for being 40 DEG C in temperature
Under part, stirring for 24 hours, obtains reaction solution；
3., revolving speed be 3500rpm under conditions of, reaction solution is centrifuged 10min, removes supernatant after centrifugation, is sunk
Starch；
4., deionized water is added into sediment, be uniformly mixed, obtain precipitated liquid, ultrasonic power be 750W condition
Under, by precipitated liquid ultrasound 15min, it then is centrifuged 10min under conditions of revolving speed is 3500rpm, removes supernatant, obtained primary
Sediment after washing；
The quality of the sediment and the volume ratio of deionized water are 1g:40mL；
5., 4. the sediment after once washing repeated by step, until supernatant pH is 5, the precipitating after being washed
Object；
6., into the sediment after washing ethyl alcohol is added, obtain mixed solution B, under conditions of ultrasonic power is 750W,
To mixed solution B ultrasound sound 1h, it then is centrifuged 15min under conditions of revolving speed is 10000rpm, the lower layer after obtaining ethyl alcohol cleaning
Sediment；
The percentage by volume of sediment after washing in the mixed solution B is 8%；
7., into the lower sediment thing after ethyl alcohol cleaning deionized water is added, be uniformly mixed, obtain mixed solution C, super
Under conditions of acoustical power is 750W, to mixed solution C ultrasound 30min, then it is centrifuged under conditions of revolving speed is 3500rpm
2min takes black rice-pudding color upper liquid dry, obtains MXene-Ti3C2, by MXene-Ti3C2It is mixed with water, obtains MXene-Ti3C2Dispersion
Liquid；The MXene-Ti3C2Dispersion liquid concentration is 14mg/mL；
The percentage by volume of lower sediment thing in the mixed solution C after ethyl alcohol cleaning is 2%；
Three, 20mL selenium-hydrazine hydrate dispersion liquid and 10mL cetyl trimethylammonium bromide solution are mixed and magnetic force stirs
It mixes, then under conditions of reaction temperature is 200 DEG C, reacts 12h, obtain mixed solution D；
Four, mixed solution D deionized water and ethyl alcohol are cleaned and is centrifuged, finally under conditions of temperature is 50 DEG C, very
Sky drying 4h, obtains MoSe2@MXene-Ti3C2Composite material completes a kind of selenizing molybdenum two-dimensional layer carbonization titanium composite material
Preparation method.
To MoSe manufactured in the present embodiment2@MXene-Ti3C2Composite material carries out morphology characterization and electrochemical property test.
Fig. 1 is MoSe prepared by embodiment one2@MXene-Ti3C2The transmission electron microscopy figure of composite material, as seen from the figure,
MoSe manufactured in the present embodiment2@MXene-Ti3C2Composite material has spherical micro nano structure, and the diameter of big ball is 800nm,
MoSe2It is distributed in micro-nano ball surface, specific surface area with higher can effectively increase active site and load capacity.
Fig. 2 is MoSe2@MXene-Ti3C2And MoSe2Linear scan curve graph, 1 is MoSe2, 2 prepare for embodiment one
MoSe2@MXene-Ti3C2Composite material；It is tested in alkaline electrolyte, electrolyte is 1mol/LKOH solution, current density
For 10mA/cm2When, MoSe2Overpotential is 360mV, and MoSe2@MXene-Ti3C2Overpotential be 260mV, the addition of MXene
It is substantially reduced the overpotential of evolving hydrogen reaction.
Claims (10)
1. a kind of preparation method of selenizing molybdenum two-dimensional layer carbonization titanium composite material, it is characterised in that a kind of selenizing molybdenum two-dimensional layer
The preparation method of carbonization titanium composite material carries out according to the following steps:
One, 12h~for 24 hours is mixed in the hydrazine hydrate that Se powder and mass percent are 97%~98%, obtains selenium-hydrazine hydrate
Dispersion liquid；
The volume ratio of mole hydrazine hydrate for being 97%~98% with mass percent of the Se powder is (0.8~1.3) mmol:
5mL；
Two, by MXene-Ti3C2Dispersion liquid is mixed with cetyl trimethylammonium bromide, the condition for being 30 DEG C~50 DEG C in temperature
Under, 0.5h~2h is stirred, sodium molybdate is added and stirs 0.2h~2h, obtains cetyl trimethylammonium bromide solution；
The MXene-Ti3C2The volume of dispersion liquid and the mass ratio of cetyl trimethylammonium bromide are (10~50) mL:
1g；The MXene-Ti3C2The volume of dispersion liquid and the molar ratio of sodium molybdate are (10~15) mL:1mmol；
The MXene-Ti3C2Dispersion liquid carries out according to the following steps: 1., by lithium fluoride and concentration be 8.5mol/L~
The mixed in hydrochloric acid of 9.5mol/L simultaneously stirs 25min~35min, obtains mixed solution A；
The volume ratio for the hydrochloric acid that the quality and concentration of the lithium fluoride are 8.5mol/L~9.5mol/L is 1g:(30~50)
mL；
2., with the speed of 1mL/s~3mL/s, by MAX-Ti3AlC2It is added in mixed solution A, is 35 DEG C~45 DEG C in temperature
Under conditions of, stirring 20h~for 24 hours, obtain reaction solution；
The MAX-Ti3AlC2Quality and mixed solution A volume ratio be 1g:(10~20) mL；
3., revolving speed be 3000rpm~4000rpm under conditions of, by reaction solution be centrifuged 8min~12min, remove after centrifugation on
Clear liquid obtains sediment；
4., deionized water is added into sediment, be uniformly mixed, obtain precipitated liquid, ultrasonic power be 700W~800W item
Under part, by precipitated liquid ultrasound 10min~20min, then revolving speed be 3000rpm~4000rpm under conditions of centrifugation 5min~
15min removes supernatant, the sediment after obtaining once washing；
The quality of the sediment and the volume ratio of deionized water are 1g:(30~40) mL；
5., 4. the sediment after once washing repeated by step, until supernatant pH is 4~5, the precipitating after being washed
Object；
6., into the sediment after washing ethyl alcohol is added, mixed solution B is obtained, in the condition that ultrasonic power is 700W~800W
Under, to mixed solution B ultrasound sound 0.8h~1.2h, then revolving speed be 8000rpm~10000rpm under conditions of centrifugation 10min~
15min, the lower sediment thing after obtaining ethyl alcohol cleaning；
The percentage by volume of sediment after washing in the mixed solution B is 5%~10%；
7., to ethyl alcohol cleaning after lower sediment thing in deionized water is added, be uniformly mixed, mixed solution C is obtained, in ultrasonic function
Rate be 700W~800W under conditions of, to mixed solution C ultrasound 20min~30min, then revolving speed be 3000rpm~
It is centrifuged 2min~4min under conditions of 4000rpm, takes black rice-pudding color upper liquid dry, obtains MXene-Ti3C2, by MXene-Ti3C2With
Water mixing, obtains MXene-Ti3C2Dispersion liquid；The MXene-Ti3C2Dispersion liquid concentration is 10mg/mL~15mg/mL；
The percentage by volume of lower sediment thing in the mixed solution C after ethyl alcohol cleaning is 2%~2.5%；
Three, selenium-hydrazine hydrate dispersion liquid and cetyl trimethylammonium bromide solution are mixed into simultaneously magnetic agitation, then reacted
Under conditions of temperature is 160 DEG C~200 DEG C, 8h~16h is reacted, mixed solution D is obtained；
The volume ratio of selenium-hydrazine hydrate dispersion liquid and cetyl trimethylammonium bromide solution is (1.6~2.2): 1；
Four, mixed solution D deionized water and ethyl alcohol are cleaned and is centrifuged, finally under conditions of temperature is 30 DEG C~50 DEG C,
Vacuum drying 1h~5h, obtains MoSe2@MXene-Ti3C2It is multiple to complete a kind of selenizing molybdenum two-dimensional layer titanium carbide for composite material
The preparation method of condensation material.
2. a kind of preparation method of selenizing molybdenum two-dimensional layer carbonization titanium composite material according to claim 1, feature exist
In Se powder described in step 1 mole hydrazine hydrate for being 97%~98% with mass percent volume ratio be (0.8~1)
mmol:5mL。
3. a kind of preparation method of selenizing molybdenum two-dimensional layer carbonization titanium composite material according to claim 1, feature exist
MXene-Ti described in step 23C2The mass ratio of the volume of dispersion liquid and cetyl trimethylammonium bromide be (10~
40)mL:1g；MXene-Ti described in step 23C2The volume of dispersion liquid and the molar ratio of sodium molybdate are (10~12) mL:
1mmol。
4. a kind of preparation method of selenizing molybdenum two-dimensional layer carbonization titanium composite material according to claim 1, feature exist
By MXene-Ti in step 23C2Dispersion liquid is mixed with cetyl trimethylammonium bromide, the item for being 30 DEG C~45 DEG C in temperature
Under part, 1h~2h is stirred, sodium molybdate is added and stirs 1h~2h, obtains cetyl trimethylammonium bromide solution.
5. a kind of preparation method of selenizing molybdenum two-dimensional layer carbonization titanium composite material according to claim 1, feature exist
In step 2 1. in by mixed in hydrochloric acid that lithium fluoride and concentration are 8.5mol/L~9mol/L and stir 25min~30min, obtain
Mixed solution A；The volume ratio for the hydrochloric acid that the quality of the lithium fluoride and concentration are 8.5mol/L~9mol/L be 1g:(30~
40)mL。
6. a kind of preparation method of selenizing molybdenum two-dimensional layer carbonization titanium composite material according to claim 1, feature exist
In step 2 2. in the speed of 1mL/s~2mL/s, by MAX-Ti3AlC2Be added in mixed solution A, temperature be 35 DEG C~
Under conditions of 40 DEG C, stirring 22h~for 24 hours, obtain reaction solution；The MAX-Ti3AlC2Quality and mixed solution A volume
Than for 1g:(15~20) mL.
7. a kind of preparation method of selenizing molybdenum two-dimensional layer carbonization titanium composite material according to claim 1, feature exist
In step 2 4. in deionized water is added into sediment, be uniformly mixed, obtain precipitated liquid, ultrasonic power be 750W~800W
Under conditions of, then precipitated liquid ultrasound 15min~20min is centrifuged under conditions of revolving speed is 3500rpm~4000rpm
5min~10min removes supernatant, the sediment after obtaining once washing；The quality of the sediment and deionized water
Volume ratio is 1g:(35~40) mL.
8. a kind of preparation method of selenizing molybdenum two-dimensional layer carbonization titanium composite material according to claim 1, feature exist
In step 2 6. in into the sediment after washing ethyl alcohol is added, obtain mixed solution B, be 750W~800W's in ultrasonic power
Under the conditions of, to mixed solution B ultrasound sound 1h~1.2h, 12min then is centrifuged under conditions of revolving speed is 9000rpm~10000rpm
~15min, the lower sediment thing after obtaining ethyl alcohol cleaning；The volume basis of sediment after being washed in the mixed solution B
Number is 5%~8%.
9. a kind of preparation method of selenizing molybdenum two-dimensional layer carbonization titanium composite material according to claim 1, feature exist
In step 2 7. in ethyl alcohol cleaning after lower sediment thing in deionized water is added, be uniformly mixed, obtain mixed solution C,
It is then 3500rpm in revolving speed to mixed solution C ultrasound 25min~30min under conditions of ultrasonic power is 750W~800W
It is centrifuged 2min~3min under conditions of~4000rpm, takes black rice-pudding color upper liquid dry, obtains MXene-Ti3C2, by MXene-Ti3C2
It is mixed with water, obtains MXene-Ti3C2Dispersion liquid；The MXene-Ti3C2Dispersion liquid concentration is 10mg/mL~14mg/mL.
10. a kind of preparation method of selenizing molybdenum two-dimensional layer carbonization titanium composite material according to claim 1, feature exist
In step 3 is by selenium-hydrazine hydrate dispersion liquid and cetyl trimethylammonium bromide solution mixes and magnetic agitation, then anti-
Answer temperature be 180 DEG C~200 DEG C under conditions of, react 8h~12h, obtain mixed solution D；Selenium-hydrazine hydrate dispersion
The volume ratio of liquid and cetyl trimethylammonium bromide solution is (1.6~2): 1.
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