CN104817083A - Rapid-heating-assisted ultrasonic stripping method for two-dimensional nanometer Ti3C2 lamella - Google Patents

Rapid-heating-assisted ultrasonic stripping method for two-dimensional nanometer Ti3C2 lamella Download PDF

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CN104817083A
CN104817083A CN201510271236.3A CN201510271236A CN104817083A CN 104817083 A CN104817083 A CN 104817083A CN 201510271236 A CN201510271236 A CN 201510271236A CN 104817083 A CN104817083 A CN 104817083A
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lamella
powder
dimensional nano
rapid heating
peels
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段小明
孙亚建
贾德昌
刘博慧
周玉
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

The invention discloses a rapid-heating-assisted ultrasonic stripping method for a two-dimensional nanometer Ti3C2 lamella, relates to a method for stripping a two-dimensional nanometer Ti3C2 lamella, and aims at solving the problem of poor stripping effect of the existing method for stripping the two-dimensional nanometer Ti3C2 lamella. The method comprises the steps of firstly, preparing Ti3AlC2 powder; secondly, preparing stacked lamellar Ti3C2Tx powder, and then, immediately placing the stacked lamellar Ti3C2Tx powder into a thermal treatment furnace after vacuumizing; then, adding the powder in a pipe into an organic solvent after cooling, and centrifuging after stirring to obtain a solid substance; and vibrating and dispersing after adding deionized water into the solid substance, filtering to obtain a powdery sample, and drying to obtain the two-dimensional nanometer Ti3C2 lamella. The ratio of single-layer or n-layer nano lamellas in the two-dimensional nanometer Ti3C2 lamella stripped by using the method disclosed by the invention is relatively high (n<10). The rapid-heating-assisted ultrasonic stripping method for the two-dimensional nanometer Ti3C2 lamella is applied to the fields of synthesis and preparation of nano ceramic materials.

Description

A kind of rapid heating assisting ultrasonic peels off two-dimensional nano Ti 3c 2the method of lamella
Technical field
The present invention relates to a kind of stripping two-dimensional nano Ti 3c 2the method of lamella.
Background technology
Two-dimensional material Ti 3c 2more more stable than Graphene.To Ti 3c 2the first-principles calculations carried out shows to have very high Young's modulus when its reference plane stretches, and flexural strength is higher than the Graphene of same thickness, and nearly Fermi's energy state density is its presoma MAX phase (Ti 3alC 2) 2.5 ~ 4.5 times.Utilize the MXene that the etchant process MAX phases such as HF obtain with functional groups such as F, OH, O, the existence of these functional groups can change the characteristic electron of MXene.Theoretical Calculation shows the Ti with F and OH functional group 3c 2show obvious characteristic of semiconductor, and the magnetic MXene sill of tool can be obtained by the kind of suitable finishing and controlled modification functional group and degree.
Ti 3c 2as a kind of New Two Dimensional material, there is uniqueness and the mechanics of excellence, electronics, magnetic performance, there is important using value.If the technical barrier of low cost, extensive preparation MXene material is resolved, the progress in the fields such as new energy materials, structured material, lubricant and electronic material must be contributed to.But prepare high quality Ti at present 3c 2still there is key issue much urgently to be resolved hurrily, such as number of plies controllability is not high, lack of homogeneity, crystalline size are little.
The ultrasonic stripping of liquid phase extensively adopted at present erodes Ti by certain density hydrofluoric acid exactly 3alC 2in Al element, then by ultrasonic disperse, obtain the Ti with functional group (F, OH) 3c 2.But due to Ti 3alC 2it is different that middle Al atomic shell and hydrofluoric acid contact situation, each lamella is caused to corrode uneven, and still have stronger combination between each synusia after corrosion, be difficult to obtain good peeling effect by means of only subsequent ultrasonic process, in products therefrom, major part remains the multilayer Ti3C2 sheet adhered to each other, and individual layer or the proportion shared by which floor nanometer sheet little.
Summary of the invention
The present invention will solve existing method to peel off two-dimensional nano Ti 3c 2the problem of the peeling effect difference of lamella, provides a kind of rapid heating assisting ultrasonic and peels off two-dimensional nano Ti 3c 2the method of lamella.
A kind of rapid heating assisting ultrasonic of the present invention peels off two-dimensional nano Ti 3c 2the method of lamella, completes according to the following steps:
One, by Ti, Al, C massage you than for 3:(1 ~ 1.1): after the ratio mixing of 2, by pressureless sintering under the condition of 1400 DEG C ~ 1500 DEG C, obtain Ti 3alC 2phase ceramics, crosses 400 orders after then being pulverized, obtains Ti 3alC 2powder;
Two, by Ti 3alC 2powder puts into hydrofluoric acid corrosion 4 ~ 24h that concentration is 20wt.% ~ 50wt.%, then adds deionized water centrifugal treating, removes liquid phase, then solid phase dried, obtain the lamellar Ti of stacking 3c 2t xpowder;
Three, by the lamellar Ti of stacking 3c 2t xpowder loads in quartz glass tube, vacuumizes the rear enclosed mouth of pipe, keeps in the heat treatment furnace of constant temperature at being then placed in 600 ~ 1200 DEG C immediately, takes out after insulation 0.5 ~ 3min;
Four, the operating process of step 3 is repeated 0 ~ 10 time;
Five, the quartz glass tube after step 4 process being cooled to room temperature, powder in take-off pipe, is then 1:(10 ~ 100 in powder and organic solvent mass ratio) ratio, powder is joined in organic solvent, centrifugal after stirring at room temperature, remove liquid phase, obtain solid formation;
Six, deionized water is added in the solid formation obtained to step 5, the mass ratio of solid formation and deionized water is 1:(200 ~ 1000), then ultrasonic generator concussion dispersion is put into, ultrasonic power is 300 ~ 800W, ultrasonic time is 2 ~ 24h, then filtered by porous anodic alumina films and obtain powdered sample, then dry at 80 ~ 200 DEG C, obtain two-dimensional nano Ti 3c 2lamella, namely completes.
The invention discloses a kind of by rapid heating assisting ultrasonic stripping two-dimensional nano Ti 3c 2the method of lamella.First, Ti, Al, C powder is synthesized Ti by pressureless sintering 3alC 2phase; Erode Al element wherein by hydrofluoric acid again, now can form the Ti adhered to each other 3c 2nanometer sheet; By its rapid heating under vacuum, the solvent adsorbed is volatilized fast, and under thermal shocking effect, destroy remaining M-A key between synusia, effectively reduce the adhesive power between synusia, significantly improve layered effect, expand lamellar spacing; Which floor afterwards again by its ultrasonic disperse in organic solvent, can be formed containing individual layer or two-dimensional nano Ti 3c 2lamella solution, can obtain two-dimensional nano Ti by suction filtration 3c 2lamella.To adopt after rapid heating ultrasonic disperse can ultrasonic stripping synusia effectively in present method, obtain than by means of only the better effect of ultrasonic disperse, and realize that technique is simple, efficiency is high, there are stronger promotion and application and be worth.Adopt the two-dimensional nano Ti that present method is peeled off 3c 2individual layer or the proportion shared by n layer nanometer sheet comparatively large (n < 10) in lamella.
Accompanying drawing explanation
Fig. 1 is that test 1 test group peels off two-dimensional nano Ti 3c 2the SEM result figure of lamella;
Fig. 2 is that test 1 control group peels off two-dimensional nano Ti 3c 2the SEM result figure of lamella.
Embodiment
Embodiment one: a kind of rapid heating assisting ultrasonic of present embodiment peels off two-dimensional nano Ti 3c 2the method of lamella, completes according to the following steps:
One, by Ti, Al, C massage you than for 3:(1 ~ 1.1): after the ratio mixing of 2, by pressureless sintering under the condition of 1400 DEG C ~ 1500 DEG C, obtain Ti 3alC 2phase ceramics, crosses 400 orders after then being pulverized, obtains Ti 3alC 2powder;
Two, by Ti 3alC 2powder puts into hydrofluoric acid corrosion 4 ~ 24h that concentration is 20wt.% ~ 50wt.%, then adds deionized water centrifugal treating, removes liquid phase, then solid phase dried, obtain the lamellar Ti of stacking 3c 2t xpowder;
Three, by the lamellar Ti of stacking 3c 2t xpowder loads in quartz glass tube, vacuumizes the rear enclosed mouth of pipe, keeps in the heat treatment furnace of constant temperature at being then placed in 600 ~ 1200 DEG C immediately, takes out after insulation 0.5 ~ 3min;
Four, the operating process of step 3 is repeated 0 ~ 10 time;
Five, the quartz glass tube after step 4 process being cooled to room temperature, powder in take-off pipe, is then 1:(10 ~ 100 in powder and organic solvent mass ratio) ratio, powder is joined in organic solvent, centrifugal after stirring at room temperature, remove liquid phase, obtain solid formation;
Six, deionized water is added in the solid formation obtained to step 5, the mass ratio of solid formation and deionized water is 1:(200 ~ 1000), then ultrasonic generator concussion dispersion is put into, ultrasonic power is 300 ~ 800W, ultrasonic time is 2 ~ 24h, then filtered by porous anodic alumina films and obtain powdered sample, then dry at 80 ~ 200 DEG C, obtain two-dimensional nano Ti 3c 2lamella, namely completes.
The meaning of present embodiment step 3 " be placed in immediately at 600 ~ 1200 DEG C and keep the heat treatment furnace of constant temperature " is be placed in the heat treatment furnace keeping constant temperature at 600 ~ 1200 DEG C at short notice.
In present embodiment, porous anodic alumina films is 47 mm dias, the WhatmanAnodisc pellumina of 0.2 μm of hole.
Present embodiment discloses a kind of by rapid heating assisting ultrasonic stripping two-dimensional nano Ti 3c 2the method of lamella.First, Ti, Al, C powder is synthesized Ti by pressureless sintering 3alC 2phase; Erode Al element wherein by hydrofluoric acid again, now can form the Ti adhered to each other 3c 2nanometer sheet; By its rapid heating under vacuum, the solvent adsorbed is volatilized fast, and under thermal shocking effect, destroy remaining M-A key between synusia, effectively reduce the adhesive power between synusia, significantly improve layered effect, expand lamellar spacing; Which floor afterwards again by its ultrasonic disperse in organic solvent, can be formed containing individual layer or two-dimensional nano Ti 3c 2lamella solution, can obtain two-dimensional nano Ti by suction filtration 3c 2lamella.To adopt after rapid heating ultrasonic disperse can ultrasonic stripping synusia effectively in present method, obtain than by means of only the better effect of ultrasonic disperse, and realize that technique is simple, efficiency is high, there are stronger promotion and application and be worth.Adopt the two-dimensional nano Ti that present method is peeled off 3c 2individual layer or the proportion shared by n layer nanometer sheet comparatively large (n < 10) in lamella.
Embodiment two: present embodiment and embodiment one unlike: speed centrifugal described in step 2 is 3500r/min.Other steps are identical with embodiment one with parameter.
Embodiment three: present embodiment and embodiment one or two unlike: the oven dry described in step 2 refers to dry 12h under 30 ~ 80 DEG C of conditions.Other steps are identical with embodiment one or two with parameter.
Embodiment four: one of present embodiment and embodiment one to three are unlike the Ti described in: step 2 and step 3 3c 2t xt in powder is-F ,-O-or-OH group, and X is the real number of 0.1 ~ 3.Other steps are identical with one of embodiment one to three with parameter.
Embodiment five: one of present embodiment and embodiment one to four unlike: vacuumizing described in step 3 refers to that being evacuated to vacuum tightness is 1.0 × 10 -3pa.Other steps are identical with one of embodiment one to four with parameter.
Embodiment six: one of present embodiment and embodiment one to five unlike: the powder described in step 5 and organic solvent mass ratio are 1:20.Other steps are identical with one of embodiment one to five with parameter.
Embodiment seven: one of present embodiment and embodiment one to six unlike: speed centrifugal described in step 5 is 3500r/min.Other steps are identical with one of embodiment one to six with parameter.
Embodiment eight: one of present embodiment and embodiment one to seven unlike: the organic solvent described in step 5 is dimethyl alum, dimethyl formamide or Triton X100.Other steps are identical with one of embodiment one to seven with parameter.
Embodiment nine: one of present embodiment and embodiment one to eight unlike: the solid formation described in step 6 and the mass ratio of deionized water are 1:500.Other steps are identical with one of embodiment one to eight with parameter.
Embodiment ten: one of present embodiment and embodiment one to nine unlike: the ultrasonic power described in step 6 is 300 ~ 800W, ultrasonic time 6h.Other steps are identical with one of embodiment one to nine with parameter.
By following verification experimental verification beneficial effect of the present invention:
Two-dimensional nano Ti is peeled off in test 1, this test test group rapid heating assisting ultrasonic 3c 2the method of lamella, completes according to the following steps:
One, after you mix than the ratio for 3:1.1:2 by Ti, Al, C massage, by pressureless sintering under the condition of 1400 DEG C, Ti is obtained 3alC 2phase ceramics, crosses 400 orders after then being pulverized, obtains Ti 3alC 2powder;
Two, by Ti 3alC 2it is that the hydrofluoric acid of 30wt.% corrodes 4h that powder puts into concentration, then adds deionized water, then under 3500r/min condition centrifugal treating, remove liquid phase, then solid phase dried, obtain the lamellar Ti of stacking 3c 2t xpowder;
Three, by the lamellar Ti of stacking 3c 2t xpowder loads in quartz glass tube, is evacuated to 1.0 × 10 -3the rear enclosed mouth of pipe, keeps at being then placed in 1100 DEG C immediately in the heat treatment furnace of constant temperature, takes out after insulation 1min;
Four, the operating process of step 3 is repeated 2 times;
Five, the quartz glass tube after step 4 process being cooled to room temperature, powder in take-off pipe, is then the ratio of 1:20 in powder and organic solvent mass ratio, powder is joined in organic solvent, centrifugal under 3500r/min condition after stirring at room temperature, remove liquid phase, obtain solid formation;
Six, deionized water is added in the solid formation obtained to step 5, the mass ratio of solid formation and deionized water is 1:500, then ultrasonic generator concussion dispersion is put into, ultrasonic power is 300 ~ 800W, ultrasonic time is 6h, then filtered by porous anodic alumina films and obtain powdered sample, then dry at 80 DEG C, obtain two-dimensional nano Ti 3c 2lamella, namely completes.
Control group peels off two-dimensional nano Ti 3c 2the method of lamella is:
One, after you mix than the ratio for 3:1.1:2 by Ti, Al, C massage, by pressureless sintering under the condition of 1400 DEG C, Ti is obtained 3alC 2phase ceramics, crosses 400 orders after then being pulverized, obtains Ti 3alC 2powder;
Two, by Ti 3alC 2it is that the hydrofluoric acid of 30wt.% corrodes 4h that powder puts into concentration, then adds deionized water, then under 3500r/min condition centrifugal treating, remove liquid phase, then solid phase dried, obtain the lamellar Ti of stacking 3c 2t xpowder;
Three, be the ratio of 1:20 in powder and organic solvent mass ratio, powder joined in organic solvent, centrifugal under 3500r/min condition after stirring at room temperature, remove liquid phase, obtain solid formation;
Six, deionized water is added in the solid formation obtained to step 5, the mass ratio of solid formation and deionized water is 1:500, then ultrasonic generator concussion dispersion is put into, ultrasonic power is 300 ~ 800W, ultrasonic time is 6h, then filtered by porous anodic alumina films and obtain powdered sample, then dry at 80 DEG C, obtain two-dimensional nano Ti 3c 2lamella, namely completes.
The test group of this test and control group peel off two-dimensional nano Ti 3c 2by Fig. 1 and Fig. 2 is known, the SEM result figure of lamella as depicted in figs. 1 and 2, can find out that test group layered effect and synusia distance are obviously better than control group.
Two-dimensional nano Ti is peeled off in test 2, this test test group rapid heating assisting ultrasonic 3c 2the method of lamella, completes according to the following steps:
One, after you mix than the ratio for 3:1.1:2 by Ti, Al, C massage, by pressureless sintering under the condition of 1400 DEG C, Ti is obtained 3alC 2phase ceramics, crosses 400 orders after then being pulverized, obtains Ti 3alC 2powder;
Two, by Ti 3alC 2it is that the hydrofluoric acid of 30wt.% corrodes 4h that powder puts into concentration, then adds deionized water, then under 3500r/min condition centrifugal treating, remove liquid phase, then solid phase dried, obtain the lamellar Ti of stacking 3c 2t xpowder;
Three, by the lamellar Ti of stacking 3c 2t xpowder loads in quartz glass tube, is evacuated to 1.0 × 10 -3the rear enclosed mouth of pipe, keeps at being then placed in 1100 DEG C immediately in the heat treatment furnace of constant temperature, takes out after insulation 0.5min;
Four, the operating process of step 3 is repeated 0 time;
Five, the quartz glass tube after step 4 process being cooled to room temperature, powder in take-off pipe, is then the ratio of 1:20 in powder and dimethyl alum mass ratio, powder is joined in dimethyl alum, centrifugal under 3500r/min condition after stirring at room temperature, remove liquid phase, obtain solid formation;
Six, deionized water is added in the solid formation obtained to step 5, the mass ratio of solid formation and deionized water is 1:500, then ultrasonic generator concussion dispersion is put into, ultrasonic power is 300 ~ 800W, ultrasonic time is 6h, then filtered by porous anodic alumina films and obtain powdered sample, then dry at 80 DEG C, obtain two-dimensional nano Ti 3c 2lamella, namely completes.
Two-dimensional nano Ti is peeled off in test 3, this test test group rapid heating assisting ultrasonic 3c 2the method of lamella, completes according to the following steps:
One, after you mix than the ratio for 3:1.1:2 by Ti, Al, C massage, by pressureless sintering under the condition of 1400 DEG C, Ti is obtained 3alC 2phase ceramics, crosses 400 orders after then being pulverized, obtains Ti 3alC 2powder;
Two, by Ti 3alC 2it is that the hydrofluoric acid of 30wt.% corrodes 4h that powder puts into concentration, then adds deionized water, then under 3500r/min condition centrifugal treating, remove liquid phase, then solid phase dried, obtain the lamellar Ti of stacking 3c 2t xpowder;
Three, by the lamellar Ti of stacking 3c 2t xpowder loads in quartz glass tube, is evacuated to 1.0 × 10 -3the rear enclosed mouth of pipe, keeps at being then placed in 1100 DEG C immediately in the heat treatment furnace of constant temperature, takes out after insulation 1min;
Four, the operating process of step 3 is repeated 0 time;
Five, the quartz glass tube after step 4 process being cooled to room temperature, powder in take-off pipe, is then the ratio of 1:20 in powder and organic solvent mass ratio, powder is joined in organic solvent, centrifugal under 3500r/min condition after stirring at room temperature, remove liquid phase, obtain solid formation;
Six, deionized water is added in the solid formation obtained to step 5, the mass ratio of solid formation and deionized water is 1:500, then ultrasonic generator concussion dispersion is put into, ultrasonic power is 300 ~ 800W, ultrasonic time is 6h, then filtered by porous anodic alumina films and obtain powdered sample, then dry at 80 DEG C, obtain two-dimensional nano Ti 3c 2lamella, namely completes.
Two-dimensional nano Ti is peeled off in test 4, this test test group rapid heating assisting ultrasonic 3c 2the method of lamella, completes according to the following steps:
One, after you mix than the ratio for 3:1.1:2 by Ti, Al, C massage, by pressureless sintering under the condition of 1400 DEG C, Ti is obtained 3alC 2phase ceramics, crosses 400 orders after then being pulverized, obtains Ti 3alC 2powder;
Two, by Ti 3alC 2it is that the hydrofluoric acid of 30wt.% corrodes 4h that powder puts into concentration, then adds deionized water, then under 3500r/min condition centrifugal treating, remove liquid phase, then solid phase dried, obtain the lamellar Ti of stacking 3c 2t xpowder;
Three, by the lamellar Ti of stacking 3c 2t xpowder loads in quartz glass tube, is evacuated to 1.0 × 10 -3the rear enclosed mouth of pipe, keeps at being then placed in 1100 DEG C immediately in the heat treatment furnace of constant temperature, takes out after insulation 3min;
Four, the operating process of step 3 is repeated 0 time;
Five, the quartz glass tube after step 4 process being cooled to room temperature, powder in take-off pipe, is then the ratio of 1:20 in powder and organic solvent mass ratio, powder is joined in organic solvent, centrifugal under 3500r/min condition after stirring at room temperature, remove liquid phase, obtain solid formation;
Six, deionized water is added in the solid formation obtained to step 5, the mass ratio of solid formation and deionized water is 1:500, then ultrasonic generator concussion dispersion is put into, ultrasonic power is 300 ~ 800W, ultrasonic time is 6h, then filtered by porous anodic alumina films and obtain powdered sample, then dry at 80 DEG C, obtain two-dimensional nano Ti 3c 2lamella, namely completes.
Two-dimensional nano Ti is peeled off in test 5, this test test group rapid heating assisting ultrasonic 3c 2the method of lamella, completes according to the following steps:
One, after you mix than the ratio for 3:1.1:2 by Ti, Al, C massage, by pressureless sintering under the condition of 1400 DEG C, Ti is obtained 3alC 2phase ceramics, crosses 400 orders after then being pulverized, obtains Ti 3alC 2powder;
Two, by Ti 3alC 2it is that the hydrofluoric acid of 30wt.% corrodes 4h that powder puts into concentration, then adds deionized water, then under 3500r/min condition centrifugal treating, remove liquid phase, then solid phase dried, obtain the lamellar Ti of stacking 3c 2t xpowder;
Three, by the lamellar Ti of stacking 3c 2t xpowder loads in quartz glass tube, is evacuated to 1.0 × 10 -3the rear enclosed mouth of pipe, keeps at being then placed in 1100 DEG C immediately in the heat treatment furnace of constant temperature, takes out after insulation 1min;
Four, the operating process of step 3 is repeated 1 time;
Five, the quartz glass tube after step 4 process being cooled to room temperature, powder in take-off pipe, is then the ratio of 1:20 in powder and organic solvent mass ratio, powder is joined in organic solvent, centrifugal under 3500r/min condition after stirring at room temperature, remove liquid phase, obtain solid formation;
Six, deionized water is added in the solid formation obtained to step 5, the mass ratio of solid formation and deionized water is 1:500, then ultrasonic generator concussion dispersion is put into, ultrasonic power is 300 ~ 800W, ultrasonic time is 6h, then filtered by porous anodic alumina films and obtain powdered sample, then dry at 80 DEG C, obtain two-dimensional nano Ti 3c 2lamella, namely completes.
Two-dimensional nano Ti is peeled off in test 6, this test test group rapid heating assisting ultrasonic 3c 2the method of lamella, completes according to the following steps:
One, after you mix than the ratio for 3:1.1:2 by Ti, Al, C massage, by pressureless sintering under the condition of 1400 DEG C, Ti is obtained 3alC 2phase ceramics, crosses 400 orders after then being pulverized, obtains Ti 3alC 2powder;
Two, by Ti 3alC 2it is that the hydrofluoric acid of 30wt.% corrodes 4h that powder puts into concentration, then adds deionized water, then under 3500r/min condition centrifugal treating, remove liquid phase, then solid phase dried, obtain the lamellar Ti of stacking 3c 2t xpowder;
Three, by the lamellar Ti of stacking 3c 2t xpowder loads in quartz glass tube, is evacuated to 1.0 × 10 -3the rear enclosed mouth of pipe, keeps at being then placed in 1100 DEG C immediately in the heat treatment furnace of constant temperature, takes out after insulation 2min;
Four, the operating process of step 3 is repeated 5 times;
Five, the quartz glass tube after step 4 process being cooled to room temperature, powder in take-off pipe, is then the ratio of 1:20 in powder and organic solvent mass ratio, powder is joined in organic solvent, centrifugal under 3500r/min condition after stirring at room temperature, remove liquid phase, obtain solid formation;
Six, deionized water is added in the solid formation obtained to step 5, the mass ratio of solid formation and deionized water is 1:500, then ultrasonic generator concussion dispersion is put into, ultrasonic power is 300 ~ 800W, ultrasonic time is 6h, then filtered by porous anodic alumina films and obtain powdered sample, then dry at 80 DEG C, obtain two-dimensional nano Ti 3c 2lamella, namely completes.
Two-dimensional nano Ti is peeled off in test 7, this test test group rapid heating assisting ultrasonic 3c 2the method of lamella, completes according to the following steps:
One, after you mix than the ratio for 3:1.1:2 by Ti, Al, C massage, by pressureless sintering under the condition of 1400 DEG C, Ti is obtained 3alC 2phase ceramics, crosses 400 orders after then being pulverized, obtains Ti 3alC 2powder;
Two, by Ti 3alC 2it is that the hydrofluoric acid of 30wt.% corrodes 4h that powder puts into concentration, then adds deionized water, then under 3500r/min condition centrifugal treating, remove liquid phase, then solid phase dried, obtain the lamellar Ti of stacking 3c 2t xpowder;
Three, by the lamellar Ti of stacking 3c 2t xpowder loads in quartz glass tube, is evacuated to 1.0 × 10 -3the rear enclosed mouth of pipe, keeps at being then placed in 1100 DEG C immediately in the heat treatment furnace of constant temperature, takes out after insulation 3min;
Four, the operating process of step 3 is repeated 10 times;
Five, the quartz glass tube after step 4 process being cooled to room temperature, powder in take-off pipe, is then the ratio of 1:20 in powder and organic solvent mass ratio, powder is joined in organic solvent, centrifugal under 3500r/min condition after stirring at room temperature, remove liquid phase, obtain solid formation;
Six, deionized water is added in the solid formation obtained to step 5, the mass ratio of solid formation and deionized water is 1:500, then ultrasonic generator concussion dispersion is put into, ultrasonic power is 300 ~ 800W, ultrasonic time is 6h, then filtered by porous anodic alumina films and obtain powdered sample, then dry at 80 DEG C, obtain two-dimensional nano Ti 3c 2lamella, namely completes.
In test 1 ~ 7, porous anodic alumina films is 47 mm dias, the WhatmanAnodisc pellumina of 0.2 μm of hole; Step 2 and the Ti described in step 3 3c 2t xt in powder is-the F ,-O-or-OH group after corrosion, powder generated, and X is the real number of 0.1 ~ 3.
Test 1 ~ 7 adopts rapid heating assisting ultrasonic to peel off, and can before ultrasonic, sheet interlayer spacing be increased, two-dimensional nano Ti 3c 2lamella is more easily separated, and production efficiency is improved, and in addition owing to adopting rapid heating assisting ultrasonic to peel off, more easily obtains individual layer or which floor two-dimensional nano Ti 3c 2sheet, makes the quality of production be improved.The two-dimensional nano Ti that test 1 ~ 7 is peeled off 3c 2individual layer or the proportion shared by n layer nanometer sheet comparatively large (n < 10) in lamella.

Claims (9)

1. a rapid heating assisting ultrasonic peels off two-dimensional nano Ti 3c 2the method of lamella, is characterized in that the method completes according to the following steps:
One, by Ti, Al, C massage you than for 3:(1 ~ 1.1): after the ratio mixing of 2, by pressureless sintering under the condition of 1400 DEG C ~ 1500 DEG C, obtain Ti 3alC 2phase ceramics, crosses 400 orders after then being pulverized, obtains Ti 3alC 2powder;
Two, by Ti 3alC 2powder puts into hydrofluoric acid corrosion 4 ~ 24h that concentration is 20wt.% ~ 50wt.%, then adds deionized water centrifugal treating, removes liquid phase, then solid phase dried, obtain the lamellar Ti of stacking 3c 2t xpowder;
Three, by the lamellar Ti of stacking 3c 2t xpowder loads in quartz glass tube, vacuumizes the rear enclosed mouth of pipe, is then placed in the heat treatment furnace of 600 ~ 1200 DEG C immediately, takes out after insulation 0.5 ~ 3min;
Four, the operating process of step 3 is repeated 0 ~ 10 time;
Five, the quartz glass tube after step 4 process being cooled to room temperature, powder in take-off pipe, is then 1:(10 ~ 100 in powder and organic solvent mass ratio) ratio, powder is joined in organic solvent, centrifugal after stirring at room temperature, remove liquid phase, obtain solid formation;
Six, deionized water is added in the solid formation obtained to step 5, the mass ratio of solid formation and deionized water is 1:(200 ~ 1000), then ultrasonic generator concussion dispersion is put into, ultrasonic power is 300 ~ 800W, ultrasonic time is 2 ~ 24h, then filtered by porous anodic alumina films and obtain powdered sample, then dry at 80 ~ 200 DEG C, obtain two-dimensional nano Ti 3c 2lamella, namely completes.
2. a kind of rapid heating assisting ultrasonic according to claim 1 peels off two-dimensional nano Ti 3c 2the method of lamella, is characterized in that speed centrifugal described in step 2 is 3500r/min.
3. a kind of rapid heating assisting ultrasonic according to claim 1 peels off two-dimensional nano Ti 3c 2the method of lamella, is characterized in that the oven dry described in step 2 refers to dry 12h under 30 ~ 80 DEG C of conditions.
4. a kind of rapid heating assisting ultrasonic according to claim 1 peels off two-dimensional nano Ti 3c 2the method of lamella, is characterized in that the Ti described in step 2 and step 3 3c 2t xt in powder is-F ,-O-or-OH group, and X is the real number of 0.1 ~ 3.
5. a kind of rapid heating assisting ultrasonic according to claim 1 peels off two-dimensional nano Ti 3c 2the method of lamella, is characterized in that vacuumizing described in step 3 refers to that being evacuated to vacuum tightness is 1.0 × 10 -3pa.
6. a kind of rapid heating assisting ultrasonic according to claim 1 peels off two-dimensional nano Ti 3c 2the method of lamella, is characterized in that powder described in step 5 and organic solvent mass ratio are 1:20.
7. a kind of rapid heating assisting ultrasonic according to claim 1 peels off two-dimensional nano Ti 3c 2the method of lamella, is characterized in that speed centrifugal described in step 5 is 3500r/min.
8. a kind of rapid heating assisting ultrasonic according to claim 1 peels off two-dimensional nano Ti 3c 2the method of lamella, is characterized in that the organic solvent described in step 5 is dimethyl alum, dimethyl formamide or Triton X100.
9. a kind of rapid heating assisting ultrasonic according to claim 1 peels off two-dimensional nano Ti 3c 2the method of lamella, is characterized in that the mass ratio of solid formation described in step 6 and deionized water is 1:500.
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CN105098162A (en) * 2015-09-14 2015-11-25 哈尔滨工业大学 Preparation method for titanium carbide nanosheet/graphene composite material capable of being used as anode of lithium ion battery
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
CN105253886A (en) * 2015-10-28 2016-01-20 常州轻工职业技术学院 Preparation method and application of TiC nanosheet
CN106048711A (en) * 2016-05-30 2016-10-26 哈尔滨师范大学 Method for synthesizing two-dimensional ultrathin single-crystal Ti3C2Tx lamella
CN106178979A (en) * 2016-08-31 2016-12-07 华南理工大学 High-performance two-dimensional stratiform Ti3c2mXene film and preparation method thereof and the application in water process
CN106315669A (en) * 2016-08-30 2017-01-11 陕西科技大学 Preparation method of two-dimensional Ti2AlC nanosheets
CN106430195A (en) * 2016-10-14 2017-02-22 北京大学 MXene material and preparation method and application thereof
CN106744732A (en) * 2017-01-11 2017-05-31 苏州大学 The method of green syt two dimension transition metal carbide or nitride nano piece
CN106848226A (en) * 2017-01-20 2017-06-13 西南交通大学 A kind of anisotropy titanium nitride ceramic film and preparation method thereof
CN106981633A (en) * 2017-04-10 2017-07-25 深圳市佩成科技有限责任公司 A kind of poly- anthraquinone thioether/Ti3C2Tx/ sulphur composite
CN107117616A (en) * 2017-05-27 2017-09-01 陕西科技大学 A kind of method that utilization ternary MAX material prepares stratiform MXenes materials
CN108375564A (en) * 2017-07-03 2018-08-07 天津大学 The preparation method of self-supporting stratified material MXenes and its application as Raman substrate
CN108455612A (en) * 2018-03-13 2018-08-28 广西大学 It is a kind of to prepare high-purity titanium carbide material Ti3C2TxMethod
CN108584959A (en) * 2018-05-04 2018-09-28 浙江大学 A kind of preparation method for being layered two-dimentional transition metal carbide or the carbonization Tritanium/Trititanium of carbonitride-two improving antibiotic property
CN109250718A (en) * 2017-07-13 2019-01-22 中国科学院宁波材料技术与工程研究所 A kind of removing Ti3C2The method of nanometer sheet
CN109913868A (en) * 2019-04-11 2019-06-21 陕西理工大学 A kind of hole array steel surface composite coating and preparation method thereof
CN109928393A (en) * 2019-03-12 2019-06-25 郜明文 A kind of preparation method and applications of porous two-dimentional transition metal carbide
CN110803704A (en) * 2019-11-12 2020-02-18 湖南艾威尔新能源科技有限公司 Titanium carbide-graphene composite material and preparation method and application thereof
CN111073220A (en) * 2020-01-02 2020-04-28 中国科学院兰州化学物理研究所 Self-lubricating composite material and preparation method and application thereof
CN111928500A (en) * 2020-07-21 2020-11-13 华中科技大学 Preparation method of MXene nanofluid, MXene nanofluid and solar heat collector
CN111978694A (en) * 2020-08-14 2020-11-24 华南理工大学 Polylactic acid composite material with tensile resistance and impact resistance and preparation method thereof
CN112053925A (en) * 2020-10-09 2020-12-08 深圳先进技术研究院 Field emission cathode and preparation method thereof
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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
CN105098162A (en) * 2015-09-14 2015-11-25 哈尔滨工业大学 Preparation method for titanium carbide nanosheet/graphene composite material capable of being used as anode of lithium ion battery
CN105253886A (en) * 2015-10-28 2016-01-20 常州轻工职业技术学院 Preparation method and application of TiC nanosheet
CN106048711A (en) * 2016-05-30 2016-10-26 哈尔滨师范大学 Method for synthesizing two-dimensional ultrathin single-crystal Ti3C2Tx lamella
CN106315669B (en) * 2016-08-30 2017-12-19 陕西科技大学 A kind of two-dimentional Ti2The preparation method of AlC nanometer sheets
CN106315669A (en) * 2016-08-30 2017-01-11 陕西科技大学 Preparation method of two-dimensional Ti2AlC nanosheets
CN106178979A (en) * 2016-08-31 2016-12-07 华南理工大学 High-performance two-dimensional stratiform Ti3c2mXene film and preparation method thereof and the application in water process
CN106178979B (en) * 2016-08-31 2019-04-09 华南理工大学 High-performance two-dimensional stratiform Ti3C2- MXene film and preparation method thereof and the application in water process
CN106430195A (en) * 2016-10-14 2017-02-22 北京大学 MXene material and preparation method and application thereof
CN106744732A (en) * 2017-01-11 2017-05-31 苏州大学 The method of green syt two dimension transition metal carbide or nitride nano piece
CN106848226A (en) * 2017-01-20 2017-06-13 西南交通大学 A kind of anisotropy titanium nitride ceramic film and preparation method thereof
CN106981633A (en) * 2017-04-10 2017-07-25 深圳市佩成科技有限责任公司 A kind of poly- anthraquinone thioether/Ti3C2Tx/ sulphur composite
CN107117616A (en) * 2017-05-27 2017-09-01 陕西科技大学 A kind of method that utilization ternary MAX material prepares stratiform MXenes materials
CN108375564A (en) * 2017-07-03 2018-08-07 天津大学 The preparation method of self-supporting stratified material MXenes and its application as Raman substrate
CN109250718A (en) * 2017-07-13 2019-01-22 中国科学院宁波材料技术与工程研究所 A kind of removing Ti3C2The method of nanometer sheet
CN108455612A (en) * 2018-03-13 2018-08-28 广西大学 It is a kind of to prepare high-purity titanium carbide material Ti3C2TxMethod
CN108584959A (en) * 2018-05-04 2018-09-28 浙江大学 A kind of preparation method for being layered two-dimentional transition metal carbide or the carbonization Tritanium/Trititanium of carbonitride-two improving antibiotic property
CN109928393A (en) * 2019-03-12 2019-06-25 郜明文 A kind of preparation method and applications of porous two-dimentional transition metal carbide
CN109928393B (en) * 2019-03-12 2021-03-30 宝晟(苏州)能源科技有限公司 Preparation method and application of porous two-dimensional transition metal carbide
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CN110803704A (en) * 2019-11-12 2020-02-18 湖南艾威尔新能源科技有限公司 Titanium carbide-graphene composite material and preparation method and application thereof
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CN113772619B (en) * 2020-06-10 2023-07-11 宝山钢铁股份有限公司 Microporous channel membrane and preparation method thereof
CN111928500A (en) * 2020-07-21 2020-11-13 华中科技大学 Preparation method of MXene nanofluid, MXene nanofluid and solar heat collector
CN111978694A (en) * 2020-08-14 2020-11-24 华南理工大学 Polylactic acid composite material with tensile resistance and impact resistance and preparation method thereof
CN111978694B (en) * 2020-08-14 2021-06-08 华南理工大学 Polylactic acid composite material with tensile resistance and impact resistance and preparation method thereof
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