CN108726519A - A method of preparing MXenes colloids using self-propagating high-temperature method synthesis MAX phase materials - Google Patents
A method of preparing MXenes colloids using self-propagating high-temperature method synthesis MAX phase materials Download PDFInfo
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Abstract
The invention discloses a kind of methods preparing MXenes colloids using self-propagating high-temperature method synthesis MAX phase materials, include the following steps：Titanium valve, aluminium powder and graphite powder are taken, vacuum electric heating drying is carried out, titanium, aluminium and the graphite powder after drying is ground mixing；Mixed-powder is added in graphite tank, is put into self-propagating high-temperature reaction kettle, reacts under an argon, by Ti3AlC2It is performed etching in etching liquid, the purees etched is washed to neutrality, and be centrifuged out purees precipitation；By Ti3C2Purees is added in deionized water in a reservoir, carries out ultrasonic disperse under argon gas atmosphere protection, the solution after ultrasound is centrifuged, Ti is prepared3C2Colloidal solution.The present invention prepares MAX phase materials using self-propagating high-temperature method, and process is simple and convenient, safety and environmental protection, takes that low, energy consumption is low, and lytic activity is high, is easy etching.The MAX phase material activity of preparation is high, is easy etching.
Description
Technical field
The invention belongs to field of material technology, more particularly to a kind of preparation method of MXenes colloids.
Background technology
Since 2010 obtain the Nobel Prize, graphene is with its unique two-dimensional structure and excellent electricity, mechanics
Performance and research hotspot as material and related field, and the research boom of two-dimensional material has been started in the world, other two
Dimension material such as hexagonal boron nitride, metal oxide and hydroxide etc. also result in the very big concern of researcher.MXenes is
A kind of two dimension transition metal carbon or/and nitride, is by the Yury of Univ Drexel of the U.S. (Drexel University)
A kind of New Two Dimensional structural material that Gogotsi professors and Michel W.Barsoum professors et al. had found in cooperation in 2011.
The chemical general formula of MXenes can use Mn+1XnTz indicates that wherein M refers to magnesium-yttrium-transition metal (such as Ti, Zr, Hf, V, Nb, Ta, Cr, Sc
Deng), X refers to C or/and N, and n is generally 1-3, and Tz refers to surface group (such as O2 -、OH-、F-、NH3、NH4 +Deng).The stripping of the material is
Using the difference of bond energy between M-A and M-C, while keeping not destroying M-C structures, the chemical bond between M-A is destroyed, makes A layers
MAX matrixes (wherein M is transition metal element, and A is the IIIth and the IVth major element, and X is C or N element) are detached from, to obtain two
Tie up stratified nano materials.These design features make MXenes have the characteristics that similar graphene high-specific surface area, high conductivity, again
It is flexibly adjustable to have component, the advantages such as minimum nanometer thickness is controllable, in electrochemical energy storage, photocatalysis, absorption, sensor, lead
The fields such as electric filler have wide application.
MAX phases are mainly realized by high temperature process heat method at present, and the preparation of MXenes colloids is usually with MAX phase materials
For raw material, performed etching using HF acid.
However, the preparation process of current MAX phase materials there is high energy consumption, time-consuming the shortcomings of.And high temperature solid-state
The MAX phase materials being synthetically prepared are often active low, it is difficult to which etching obtains MXenes colloids.
Invention content
The object of the present invention is to provide a kind of sides preparing MXenes colloids using self-propagating high-temperature method synthesis MAX phase materials
Method
To achieve the above object, the technical solution adopted by the present invention is：
A method of MXenes colloids being prepared using self-propagating high-temperature method synthesis MAX phase materials, are included the following steps：
(1) configuration of raw material：Take titanium, aluminium and powdered graphite, carry out vacuum electric heating drying, by after drying titanium, aluminium and
Graphite powder is ground mixing, obtains mixed-powder；
(2)Ti3AlC2Synthesis：The mixed-powder that step (1) is obtained is added in graphite tank, and it is anti-to be put into self-propagating high-temperature
It answers in kettle, reacts under an argon, obtain Ti3AlC2；
(3)Ti3C2The preparation of purees：Ti prepared by step (2)3AlC2It performs etching, will etch in etching liquid
Purees wash to neutrality, and be centrifuged out purees precipitation, obtain Ti3C2Purees；
(4)Ti3C2The preparation of colloid：The Ti that step (3) is obtained3C2Purees is added in deionized water in a reservoir,
Argon gas atmosphere protection is lower to carry out ultrasonic disperse, and the solution after ultrasound is centrifuged, Ti is prepared3C2Colloidal solution.
In the step (1), the molar ratio of titanium, aluminium and powdered graphite is 3：1：2.
In the step (1), vacuum electric heating drying temperature be 60~80 DEG C, the time be 12~for 24 hours.
In the step (1), ground and mixed carries out in the ball mill, and the rotating speed of ball mill is 300r/min, milling time
For 3h.
In the step (2), reaction temperature is 150~250 DEG C.
In the step (2), boron nitride is added in self-propagating high-temperature reaction kettle.
In the step (3), etching liquid is the mixed aqueous solution of HCl and LiF, wherein a concentration of 9M of HCl, LiF's is dense
Degree is 0.1g/mL；Etch period is 24~48h.
In the step (4), ultrasonic disperse is 1~4h of ultrasound at 30~40KHZ.
In the step (4), it is to centrifuge 1h under 3500r/min to centrifuge tangible rotating speed.
Advantageous effect：The present invention solves the disadvantage that traditional tube furnace sintering method, is prepared using self-propagating high-temperature method
MAX phase materials, process is simple and convenient, safety and environmental protection, takes that low, energy consumption is low, and lytic activity is high, is easy etching, prepares
Next MXenes phases colloidal stability is good, layer structure is apparent, can be carried out with other colloids or soluble material compound.
Description of the drawings
Fig. 1 is Ti in embodiment 13C2TxPattern picture of the colloid under Flied emission projection Electronic Speculum (TEM)；
Fig. 2 is in embodiment 1 to the Ti after sprawling reaction3AlC2Sintered body；
Fig. 3 is Ti in embodiment 13C2TxSelf-supporting film picture of the colloid after suction filtration and drying；
Fig. 4 is Ti in embodiment 13C2TxSelf-supporting film of the colloid after suction filtration and drying folds picture.
Specific implementation mode
Further explanation is done to the present invention with reference to embodiment.
Embodiment 1
By titanium valve, aluminium powder, graphite powder according to molar ratio 3：1：After 2 weigh, 60 DEG C of dryings in vacuum electric heating drying box
12h in the case of same day relative air humidity about 38%, is mixed in the rotating speed of QB-BP ball mills at 300r/min, grinding is stirred
Mix 3h.Self- propagating sintering is carried out after cooling, and boron nitride protection is added, control ar pressure is 1 local atmospheric pressure in reaction kettle,
Reactor temperature control is at 150~200 DEG C when reaction.Sintered sintered body picture is as shown in Figure 2.Sintered body crushing grinding
To 300 mesh, 2g Ti are taken3AlC2It is positioned in 20mL etching liquids and etches for 24 hours, wherein etching liquid is that the mixing of HCl and LiF is water-soluble
Liquid, wherein a concentration of 0.1g/mL of a concentration of 9M of HCl, LiF.Purees centrifuge washing after etching to PH be neutrality, it is special
Argon gas is passed through in fixed container as protective gas, the ultrasound 1h at 30KHZ.Under black liquor 3500r/min after ultrasound from
Heart 1h obtains black colloidal solution.TEM pictures such as Fig. 1 of black colloid.It is filtered black colloidal solution to obtain self-supporting
Film.Self-supporting film figure such as Fig. 3 and Fig. 4
From figure 1 it appears that three-dimensional MAX phase materials have successfully been prepared into two-dimensional MXenes phase materials.
As can be seen that self-supporting film has good toughness from Fig. 3, Fig. 4, and can be folded.
Embodiment 2
By titanium valve, aluminium powder, graphite powder according to molar ratio 3：1：After 2 weigh, 60 DEG C of dryings in vacuum electric heating drying box
12h in the case of same day relative air humidity about 50%, is mixed in the rotating speed of QB-BP ball mills at 300r/min, grinding is stirred
Mix 3h.Self- propagating sintering is carried out after cooling, and boron nitride protection is added, control ar pressure is 1 local atmospheric pressure in reaction kettle,
Reactor temperature control is at 200--250 DEG C when reaction.Sintered body crushing grinding takes 2g Ti to 300 mesh3AlC2It is positioned over
It is etched in 20mL etching liquids for 24 hours, wherein etching liquid is the mixed aqueous solution of HCl and LiF, wherein a concentration of 9M, LiF of HCl
A concentration of 0.1g/mL.Purees centrifuge washing after etching, to be neutral, is passed through argon gas as protection to PH in specific container
Gas, the ultrasound 1h at 30KHZ.1h is centrifuged under black liquor 3500r/min after ultrasound, obtains black colloidal solution.It will be black
Coloring agent liquid solution is filtered to obtain self-supporting film.
Embodiment 3
By titanium valve, aluminium powder, graphite powder according to molar ratio 3：1：After 2 weigh, 80 DEG C of dryings in vacuum electric heating drying box
12h in the case of same day relative air humidity about 50%, is mixed in the rotating speed of QB-BP ball mills at 400r/min, grinding is stirred
Mix 3h.Self- propagating sintering is carried out after cooling, boron nitride protection is added, and control ar pressure is 1.5 local air in reaction kettle
Pressure, reactor temperature control is at 200~250 DEG C when reaction.Sintered body crushing grinding takes 2g Ti to 300 mesh3AlC2It is positioned over
It is etched in 20mL etching liquids for 24 hours, wherein etching liquid is the mixed aqueous solution of HCl and LiF, wherein a concentration of 9M, LiF of HCl
A concentration of 0.1g/mL.Purees centrifuge washing after etching, to be neutral, is passed through argon gas as protection to PH in specific container
Gas, the ultrasound 2h at 40KHZ.1h is centrifuged under black liquor 3500r/min after ultrasound, obtains black colloidal solution.It will be black
Coloring agent liquid solution is filtered to obtain self-supporting film.
Embodiment 4
By titanium valve, aluminium powder, graphite powder according to molar ratio 3：1：After 2 weigh, 80 DEG C of dryings in vacuum electric heating drying box
For 24 hours, it in the case of same day relative air humidity about 50%, is mixed at 400r/min in the rotating speed of QB-BP ball mills, grinding is stirred
Mix 4h.Self- propagating sintering is carried out after cooling, and boron nitride protection is added, control ar pressure is 2 local atmospheric pressure in reaction kettle,
Reactor temperature control is at 200~250 DEG C when reaction.Sintered body crushing grinding takes 2g Ti to 300 mesh3AlC2It is positioned over
It is etched in 20mL etching liquids for 24 hours, wherein etching liquid is the mixed aqueous solution of HCl and LiF, wherein a concentration of 9M, LiF of HCl
A concentration of 0.1g/mL.Purees centrifuge washing after etching, to be neutral, is passed through argon gas as protection to PH in specific container
Gas, the ultrasound 4h at 40KHZ.1h is centrifuged under black liquor 3500r/min after ultrasound, obtains black colloidal solution.It will be black
Coloring agent liquid solution is filtered to obtain self-supporting film.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of method preparing MXenes colloids using self-propagating high-temperature method synthesis MAX phase materials, it is characterised in that：Including with
Lower step：
(1) configuration of raw material：Titanium valve, aluminium powder and graphite powder are taken, vacuum electric heating drying is carried out, by titanium, aluminium and the stone after drying
Ink powder is ground mixing, obtains mixed-powder；
(2)Ti3AlC2Synthesis：The mixed-powder that step (1) is obtained is added in graphite tank, is put into self-propagating high-temperature reaction kettle
In, it reacts under an argon, obtains Ti3AlC2；
(3)Ti3C2The preparation of purees：Ti prepared by step (2)3AlC2It is performed etching in etching liquid, the mud that will be etched
Shape object is washed to neutrality, and is centrifuged out purees precipitation, obtains Ti3C2Purees；
(4)Ti3C2The preparation of colloid：The Ti that step (3) is obtained3C2Purees is added in deionized water in a reservoir, in argon gas
Ultrasonic disperse is carried out under atmosphere protection, and the solution after ultrasound is centrifuged, Ti is prepared3C2Colloidal solution.
2. the method according to claim 1 for preparing MXenes colloids using self-propagating high-temperature method synthesis MAX phase materials,
It is characterized in that：In the step (1), the molar ratio of titanium, aluminium and powdered graphite is 3：1：2.
3. the method according to claim 1 for preparing MXenes colloids using self-propagating high-temperature method synthesis MAX phase materials,
It is characterized in that：In the step (1), vacuum electric heating drying temperature be 60~80 DEG C, the time be 12~for 24 hours.
4. the method according to claim 1 for preparing MXenes colloids using self-propagating high-temperature method synthesis MAX phase materials,
It is characterized in that：In the step (1), ground and mixed carries out in the ball mill, and the rotating speed of ball mill is 300r/min, milling time
For 3h.
5. the method according to claim 1 for preparing MXenes colloids using self-propagating high-temperature method synthesis MAX phase materials,
It is characterized in that：In the step (2), reaction temperature is 150~250 DEG C.
6. the method according to claim 1 for preparing MXenes colloids using self-propagating high-temperature method synthesis MAX phase materials,
It is characterized in that：In the step (2), boron nitride is added in self-propagating high-temperature reaction kettle.
7. the method according to claim 1 for preparing MXenes colloids using self-propagating high-temperature method synthesis MAX phase materials,
It is characterized in that：In the step (3), etching liquid is the mixed aqueous solution of HCl and LiF, wherein a concentration of 9M of HCl, LiF's
A concentration of 0.1g/mL；Etch period is 24~48h.
8. the method according to claim 1 for preparing MXenes colloids using self-propagating high-temperature method synthesis MAX phase materials,
It is characterized in that：In the step (4), ultrasonic disperse is 1~4h of ultrasound at 30~40KHZ.
9. the method according to claim 1 for preparing MXenes colloids using self-propagating high-temperature method synthesis MAX phase materials,
It is characterized in that：In the step (4), it is to centrifuge 1h under 3500r/min to centrifuge tangible rotating speed.
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Cited By (3)
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| CN112010305A (en) * | 2020-08-26 | 2020-12-01 | 盐城工学院 | Preparation (V, Ti)2AlC submicron flake and nanoparticle method |
| CN112938978A (en) * | 2021-03-03 | 2021-06-11 | 盐城工学院 | Preparation method of vanadium carbide nanosheet |
| CN113044842A (en) * | 2021-01-12 | 2021-06-29 | 辽宁中色新材科技有限公司 | Production process of high-purity aluminum titanium carbide |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113044842A (en) * | 2021-01-12 | 2021-06-29 | 辽宁中色新材科技有限公司 | Production process of high-purity aluminum titanium carbide |
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| CN112938978A (en) * | 2021-03-03 | 2021-06-11 | 盐城工学院 | Preparation method of vanadium carbide nanosheet |
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Application publication date: 20181102 |