CN105271231B - A kind of two-dimensional nano Ti3C2The preparation method of piece - Google Patents
A kind of two-dimensional nano Ti3C2The preparation method of piece Download PDFInfo
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- CN105271231B CN105271231B CN201510712851.3A CN201510712851A CN105271231B CN 105271231 B CN105271231 B CN 105271231B CN 201510712851 A CN201510712851 A CN 201510712851A CN 105271231 B CN105271231 B CN 105271231B
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Abstract
The invention discloses a kind of two-dimensional nano Ti3C2The preparation method of piece, using alkaline hydrothermal synthesis method by Ti3MC2(M=Si, Al) powder is prepared into two-dimensional nano Ti3C2Piece, including by Ti3MC2Ultrasound prepares suspension during (M=Si, Al) superfines is dissolved in the alkaline hydrated oxide aqueous solution, sludge is processed to obtain by hydro-thermal, it is scrubbed again, ultrasonic, separate and obtain final product product after lyophilized, the preparation method material source is simple, obtained Ti3C2For two-dimensional slice nanostructured, non-corrosiveness, good dispersion, specific surface area are up to 128.4m2/ g, conversion rate of products is high.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, and in particular to a kind of two-dimensional nano Ti3C2The preparation method of piece.
Background technology
Two-dimensional nano Ti3C2It is most commonly seen a kind of material in new class Graphene two-dimension nano materials MXenes families.
MXenes two-dimensional materials are led to for 2011 by the Yury Gogotsi and Michael Barsoum seminars of Univ Drexel of the U.S.
Over etching MAX compounds (such as Ti3AlC2Deng) obtain first.With Ti3C2For the MXenes two-dimensional materials for representing have excellent leading
Hot, the good chemical stability of conductance and electro-chemical activity, lithium ion battery, ultracapacitor, biology sensor with
And gas detection etc. field all show good application potential.
Ti is prepared at present3C2Only method be, using hydrofluoric acid solution soak Ti3AlC2Powder more than 24 hours, etching
Fall Ti3AlC2In Al atoms, then by processes such as ultrasound, ion insertion, cleanings, obtain two-dimensional nano Ti3C2Piece, such as China
The A of the patent CN 104496461 and A of CN 104016345.Due to having used the hydrofluoric acid of highly corrosive in preparation process, most
Easily attachment is fluorinated hydrogen molecule on end-product, and Ti is caused in application3C2With strong corrosivity, two-dimensional nano is limited
Ti3C2The practicality of piece.Therefore, it is necessary to explore the small synthetic route of novel easy, environmental hazard to obtain non-corrosive two
Wiener rice Ti3C2Piece.
The content of the invention
Goal of the invention：For two-dimensional nano Ti in the prior art3C2Preparation method using caused by highly corrosive hydrofluoric acid not
Environmental issue, the present invention provides a kind of environmentally friendly controllable preparation polymolecularity two-dimensional nano Ti3C2The method of piece, obtained in the method
Ti3C2Product is big two-dimensional nano piece, non-corrosiveness, good dispersion, specific surface area.
Technical scheme：To achieve the above object, the present invention uses following technical scheme：
A kind of two-dimensional nano Ti3C2The preparation method of piece, the preparation method uses alkaline hydrothermal synthesis method by Ti3MC2
Powder is prepared into two-dimensional nano Ti3C2Piece, wherein M are Si or Al.
The preparation method is comprised the following steps：
(1) Ti is prepared3MC2Superfines；
(2) the alkaline hydrated oxide aqueous solution is prepared；
(3) in the alkaline hydrated oxide aqueous solution for preparing obtained superfines addition step (2) in step (1), obtain
To the first mixed solution, and the first mixed solution is prepared into suspension；
(4) suspension obtained in step (3) is prepared into sludge；
(5) sludge in step (4) is prepared into colloidal solution；
(6) colloidal solution in step (5) is prepared into two-dimensional nano Ti3C2Piece.
Superfines in the step (1) is with Ti3MC2Powder is raw material, with stainless steel ball as ball-milling medium, ball material
Mass ratio is 5：1, it is put into ball grinder, with the rotating speed ball milling 3 hours of 300r/min on planetary ball mill.
Step (2) the neutral and alkali hydroxide aqueous solution is prepared using deionized water dissolving potassium hydroxide or NaOH
Form, concentration is 0.5-4mol/L.
Preferably, step (2) the neutral and alkali hydroxide aqueous solution is using the preparation of deionized water dissolving potassium hydroxide
Into concentration is 1mol/L.
The mass-volume concentration of the first mixed solution in the step (3) is that every 30mL alkaline hydrated oxides aqueous solution adds
Enter 1g superfines.
The first mixed solution in the step (3) is ultrasonic 1 hour at ambient temperature, is prepared into suspension.
Sludge in the step (4) is that the suspension obtained in step (3) is put into water heating kettle, is placed in baking oven
In be heated to 240 DEG C and be incubated 24 hours, supernatant liquor is poured out after cooling, that is, obtain sludge, it is standby.
The method that colloidal solution is prepared in the step (5) is that the sludge obtained in step (4) is poured into beaker, first
It is washed with deionized twice, then with absolute ethanol washing once；The alkaline hydroxide for being added after washing and being used in step (3)
The deionized water of thing aqueous solution volume equivalent is configured to the second mixed solution liquid, then the second mixed solution is surpassed at ambient temperature
Sound 3 hours, sediment separate out is obtained colloidal solution.
Two-dimensional nano Ti in the step (6)3C2Piece is that the colloidal solution of gained in step (5) is put into refrigerator freezing
After being freezed 24 hours in room, vacuum freeze-drying is prepared from placing into freeze dryer.
Beneficial effect：Compared with prior art, the present invention has the advantage that：
(1) nano material from Ti is prepared3SiC2、Ti3AlC2Start etc. simple inorganic matter, source is simple；In preparation method
Performed etching instead of traditional hydrofluoric acid using the alkaline hydrated oxide aqueous solution, corrosivity reduction, then process is peeled off, freezing can
So that the lamella Ti with nanoscale is obtained3C2Material.
(2) product prepared by the present invention is two-dimensional nano piece, non-corrosiveness, good dispersion, the specific surface area of pattern rule
Can reach 128.4m2/g。
(3) conversion rate of products of the present invention is high, and conversion ratio can reach more than 75%.
Specific embodiment
With reference to specific embodiment, the present invention is further described, and the description of specific embodiment is substantially only model
Example, without being intended to present disclosure and its application or using limiting.
Embodiment 1
(1) with Ti3SiC2Powder is raw material, and with stainless steel ball as ball-milling medium, ball material mass ratio is 5：1, it is put into ball grinder
In, according to the rotating speed ball milling 3 hours of 300r/min on planetary ball mill, obtain Ti3SiC2Superfines；
(2) it is sufficiently stirred for deionized water dissolving potassium hydroxide at room temperature, obtains potassium hydroxide aqueous solution, concentration is
1mol/L；
(3) Ti in step (1) is taken3SiC2Potassium hydroxide aqueous solution obtained in superfines addition step (2) is mixed to get
First mixed solution, wherein adding 1gTi per 30mL potassium hydroxide aqueous solutions3SiC2Superfines；The first mixed solution is existed again
Ultrasound 1 hour, obtains the suspension of muddiness at room temperature；
(4) suspension in step (3) is taken, is poured into polytetrafluoroethylliner liner, reinstalled in water heating kettle, be placed in baking oven
It is heated to 240 DEG C and is incubated 24 hours, reactor is opened after cooling, the supernatant liquor in polytetrafluoroethylliner liner is poured out,
Further take out the sludge of bottom；
(5) sludge in step (4) is taken, beaker is poured into, is first washed with deionized twice, then washed with absolute ethyl alcohol
Wash once；Added after washing and mixed with the deionized water preparation second of the potassium hydroxide aqueous solution volume equivalent used in step (3)
Solution, then ultrasonic 3 hours at ambient temperature, the sediment separate out by the second mixed solution are closed, that is, navy blue colloid is obtained molten
Liquid；
(6) take after the colloidal solution in step (5) is put into freezer compartment of refrigerator freezing 24 hours, place into true in freeze dryer
Sky is lyophilized, both obtains two-dimensional nano Ti3C2Piece.
Performance parameter：The two-dimensional nano Ti of acquisition3C2Piece is pure Ti through XRD tests3C2Phase, calculating by weight conversion ratio is
91.5%, specific surface area is 122.9m through BET tests2/g。
Embodiment 2
(1) with Ti3SiC2Powder is raw material, and with stainless steel ball as ball-milling medium, ball material mass ratio is 5：1, it is put into ball grinder
In, according to the rotating speed ball milling 3 hours of 300r/min on planetary ball mill, obtain Ti3SiC2Superfines；
(2) it is sufficiently stirred for deionized water dissolving potassium hydroxide at room temperature, obtains potassium hydroxide aqueous solution, concentration is
0.5mol/L；
(3) Ti in step (1) is taken3SiC2Potassium hydroxide aqueous solution obtained in superfines addition step (2) is mixed to get
First mixed solution, wherein adding 1gTi per 30mL potassium hydroxide aqueous solutions3SiC2Superfines；The first mixed solution is existed again
Ultrasound 1 hour, obtains the suspension of muddiness at room temperature；
(4) suspension in step (3) is taken, is poured into polytetrafluoroethylliner liner, reinstalled in water heating kettle, be placed in baking oven
It is heated to 240 DEG C and is incubated 24 hours, reactor is opened after cooling, the supernatant liquor in polytetrafluoroethylliner liner is poured out,
Further take out the sludge of bottom；
(5) sludge in step (4) is taken, beaker is poured into, is first washed with deionized twice, then washed with absolute ethyl alcohol
Wash once；The deionized water of the potassium hydroxide aqueous solution volume equivalent that addition is used with step (3) is prepared second and is mixed after washing
Solution, then ultrasonic 3 hours at ambient temperature, the sediment separate out by the second mixed solution, that is, be obtained navy blue colloidal solution；
(6) take after the colloidal solution in step (5) is put into freezer compartment of refrigerator freezing 24 hours, place into true in freeze dryer
Sky is lyophilized, both obtains two-dimensional nano Ti3C2Piece.
Performance parameter：The two-dimensional nano Ti of acquisition3C2Piece is pure Ti through XRD tests3C2Phase, calculating by weight conversion ratio is
85.2%, specific surface area is 100.7m through BET tests2/g。
Embodiment 3
(1) with Ti3SiC2Powder is raw material, and with stainless steel ball as ball-milling medium, ball material mass ratio is 5：1, it is put into ball grinder
In, according to the rotating speed ball milling 3 hours of 300r/min on planetary ball mill, obtain Ti3SiC2Superfines；
(2) it is sufficiently stirred for deionized water dissolving potassium hydroxide at room temperature, obtains potassium hydroxide aqueous solution, concentration is
4mol/L；
(3) Ti in step (1) is taken3SiC2Potassium hydroxide aqueous solution obtained in superfines addition step (2) is mixed to get
First mixed solution, wherein adding 1gTi per 30mL potassium hydroxide aqueous solutions3SiC2Superfines；The first mixed solution is existed again
Ultrasound 1 hour, obtains the suspension of muddiness at room temperature；
(4) suspension in step (3) is taken, is poured into polytetrafluoroethylliner liner, reinstalled in water heating kettle, be placed in baking oven
It is heated to 240 DEG C and is incubated 24 hours, reactor is opened after cooling, the supernatant liquor in polytetrafluoroethylliner liner is poured out,
Further take out the sludge of bottom；
(5) sludge in step (4) is taken, beaker is poured into, is first washed with deionized twice, then washed with absolute ethyl alcohol
Wash once；The deionized water of the potassium hydroxide aqueous solution volume equivalent that addition is used with step (3) is prepared second and is mixed after washing
Solution, then ultrasonic 3 hours at ambient temperature, the sediment separate out by the second mixed solution, that is, be obtained navy blue colloidal solution；
(6) take after the colloidal solution in step (5) is put into freezer compartment of refrigerator freezing 24 hours, place into true in freeze dryer
Sky is lyophilized, both obtains two-dimensional nano Ti3C2Piece.
Performance parameter：The two-dimensional nano Ti of acquisition3C2Piece is pure Ti through XRD tests3C2Phase, calculating by weight conversion ratio is
92.6%, specific surface area is 128.4m through BET tests2/g。
Embodiment 4
(1) with Ti3AlC2Powder is raw material, and with stainless steel ball as ball-milling medium, ball material mass ratio is 5：1, it is put into ball grinder
In, according to the rotating speed ball milling 3 hours of 300r/min on planetary ball mill, obtain Ti3AlC2Superfines；
(2) it is sufficiently stirred for deionized water dissolving potassium hydroxide at room temperature, obtains potassium hydroxide aqueous solution, concentration is
1mol/L；
(3) Ti in step (1) is taken3AlC2Potassium hydroxide aqueous solution obtained in superfines addition step (2) is mixed to get
First mixed solution, wherein adding 1gTi per 30mL potassium hydroxide aqueous solutions3AlC2Superfines；The first mixed solution is existed again
Ultrasound 1 hour, obtains the suspension of muddiness at room temperature；
(4) suspension in step (3) is taken, is poured into polytetrafluoroethylliner liner, reinstalled in water heating kettle, be placed in baking oven
It is heated to 240 DEG C and is incubated 24 hours, reactor is opened after cooling, the supernatant liquor in polytetrafluoroethylliner liner is poured out,
Further take out the sludge of bottom；
(5) sludge in step (4) is taken, beaker is poured into, is first washed with deionized twice, then washed with absolute ethyl alcohol
Wash once；Added after washing and mixed with the deionized water preparation second of the potassium hydroxide aqueous solution volume equivalent used in step (3)
Solution, then ultrasonic 3 hours at ambient temperature, the sediment separate out by the second mixed solution are closed, that is, navy blue colloid is obtained molten
Liquid；
(6) take after the colloidal solution in step (5) is put into freezer compartment of refrigerator freezing 24 hours, place into true in freeze dryer
Sky is lyophilized, both obtains two-dimensional nano Ti3C2Piece.
Performance parameter：The two-dimensional nano Ti of acquisition3C2Piece is pure Ti through XRD tests3C2Phase, calculating by weight conversion ratio is
81.6%, specific surface area is 106.3m through BET tests2/g。
Embodiment 5
(1) with Ti3SiC2Powder is raw material, and with stainless steel ball as ball-milling medium, ball material mass ratio is 5：1, it is put into ball grinder
In, according to the rotating speed ball milling 3 hours of 300r/min on planetary ball mill, obtain Ti3SiC2Superfines；
(2) it is sufficiently stirred for deionized water dissolving NaOH at room temperature, obtains sodium hydrate aqueous solution, concentration is
1mol/L；
(3) Ti in step (1) is taken3SiC2Sodium hydrate aqueous solution obtained in superfines addition step (2) is mixed to get
First mixed solution, wherein adding 1gTi per 30mL sodium hydrate aqueous solutions3SiC2Superfines；The first mixed solution is existed again
Ultrasound 1 hour, obtains the suspension of muddiness at room temperature；
(4) suspension in step (3) is taken, is poured into polytetrafluoroethylliner liner, reinstalled in water heating kettle, be placed in baking oven
It is heated to 240 DEG C and is incubated 24 hours, reactor is opened after cooling, the supernatant liquor in polytetrafluoroethylliner liner is poured out,
Further take out the sludge of bottom；
(5) sludge in step (4) is taken, beaker is poured into, is first washed with deionized twice, then washed with absolute ethyl alcohol
Wash once；Added after washing and mixed with the deionized water preparation second of the sodium hydrate aqueous solution volume equivalent used in step (3)
Solution, then ultrasonic 3 hours at ambient temperature, the sediment separate out by the second mixed solution are closed, that is, navy blue colloid is obtained molten
Liquid；
(6) take after the colloidal solution in step (5) is put into freezer compartment of refrigerator freezing 24 hours, place into true in freeze dryer
Sky is lyophilized, both obtains two-dimensional nano Ti3C2Piece.
Performance parameter：The two-dimensional nano Ti of acquisition3C2Piece is purer Ti through XRD tests3C2Phase, calculates by weight conversion ratio
It is 75.5%, specific surface area is 108.5m through BET tests2/g。
It should be appreciated that above example is only preferred embodiment of the invention, only it is that technology design of the invention is risen
To explanation example effect, it is not intended to limit the scope of the present invention, and those skilled in the art are not departing from skill of the present invention
In the spirit and scope of art scheme, modify and equivalent, all should fall within the scope and spirit of the invention.
Claims (8)
1. a kind of two-dimensional nano Ti3C2The preparation method of piece, it is characterised in that：The preparation method is using alkaline hydrothermal synthesis method
By Ti3MC2Powder is prepared into two-dimensional nano Ti3C2Piece, wherein M are Si or Al, and the preparation method specifically includes following steps：
(1) Ti is prepared3MC2Superfines；
(2) the alkaline hydrated oxide aqueous solution is prepared；
(3) the will be obtained during obtained superfines adds the alkaline hydrated oxide aqueous solution that step (2) is prepared in step (1)
One mixed solution, and the first mixed solution is prepared into suspension；
(4) suspension obtained in step (3) is prepared into sludge；
(5) sludge in step (4) is prepared into colloidal solution；
(6) colloidal solution in step (5) is prepared into two-dimensional nano Ti3C2Piece；
Sludge described in step (4) is that the suspension obtained in step (3) is put into water heating kettle, is placed in baking oven and adds
Heat is to 240 DEG C and is incubated 24 hours, after cooling pours out supernatant liquor, that is, obtain sludge.
2. two-dimensional nano Ti according to claim 13C2The preparation method of piece, it is characterised in that：Described in step (1)
Superfines is with Ti3MC2Powder is raw material, and with stainless steel ball as ball-milling medium, ball material mass ratio is 5：1, it is put into ball grinder
In, with the rotating speed ball milling 3 hours of 300r/min on planetary ball mill.
3. two-dimensional nano Ti according to claim 13C2The preparation method of piece, it is characterised in that：In step (2), the alkali
Property hydroxide aqueous solution is formulated using deionized water dissolving potassium hydroxide or NaOH, and concentration is 0.5-4mol/L.
4. two-dimensional nano Ti according to claim 13C2The preparation method of piece, it is characterised in that：In step (2), the alkali
Property hydroxide aqueous solution is formulated using deionized water dissolving potassium hydroxide, and concentration is 1mol/L.
5. two-dimensional nano Ti according to claim 13C2The preparation method of piece, it is characterised in that：Described in step (3)
The mass-volume concentration of one mixed solution is that every 30mL alkaline hydrated oxides aqueous solution adds 1g superfines.
6. two-dimensional nano Ti according to claim 1 or 53C2The preparation method of piece, it is characterised in that：By in step (3)
One mixed solution is ultrasonic 1 hour at ambient temperature, is prepared into suspension.
7. two-dimensional nano Ti according to claim 13C2The preparation method of piece, it is characterised in that glue described in step (5)
Liquid solution is that the sludge obtained in step (4) is poured into beaker, is first washed with deionized twice, then washed with absolute ethyl alcohol
Wash once；Added after washing and be configured to the deionized water of the alkaline hydrated oxide aqueous solution volume equivalent used in step (3)
Second mixed solution, then ultrasonic 3 hours at ambient temperature, the sediment separate out by the second mixed solution, that is, be obtained colloidal solution.
8. two-dimensional nano Ti according to claim 13C2The preparation method of piece, it is characterised in that described in step (6)
Two-dimensional nano Ti3C2Piece is after the colloidal solution of gained in step (5) is put into freezer compartment of refrigerator into freezing 24 hours, to place into
Vacuum freeze-drying is prepared from freeze dryer.
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| CN105905870B (en) * | 2016-04-15 | 2018-03-23 | 广东工业大学 | A kind of preparation method of metal oxide two-dimension nano materials |
| CN106185936A (en) * | 2016-07-08 | 2016-12-07 | 中国科学院上海硅酸盐研究所 | A kind of utilize ammonia intercalation, peel off two dimensional crystal titanium carbide nano material method |
| CN106784779B (en) * | 2016-12-19 | 2019-11-01 | 盐城工学院 | A kind of preparation method of nano lithium titanate and the preparation method of cell negative electrode material |
| CN109810562A (en) * | 2019-04-02 | 2019-05-28 | 杭州电子科技大学 | A kind of preparation method of RFID label antenna |
| CN110723737B (en) * | 2019-10-24 | 2021-01-26 | 郑州轻工业学院 | Wool ball type Ti3C2Preparation method and application of (MXene) nano material |
| WO2021102658A1 (en) * | 2019-11-25 | 2021-06-03 | 苏州大学 | Use of two-dimensional titanium carbide nanosheet in raman test and raman test substrate and test method |
| CN111232981B (en) * | 2020-01-17 | 2020-12-29 | 北京理工大学 | High lithium storage capacity Ti3C2TxMechanochemical preparation method of |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104016345A (en) * | 2014-06-03 | 2014-09-03 | 河海大学 | Method for preparing graphene-like two-dimensional laminar titanium carbide nanoplate |
| CN104192967A (en) * | 2014-08-19 | 2014-12-10 | 浙江大学 | Application of Ti3C2 nanosheet in treating high-oxidizability toxic metal ions in water |
| CN104868104A (en) * | 2015-03-27 | 2015-08-26 | 浙江工业大学 | Two-dimensional layered titanium carbide/metal ion composite material and application thereof |
-
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104016345A (en) * | 2014-06-03 | 2014-09-03 | 河海大学 | Method for preparing graphene-like two-dimensional laminar titanium carbide nanoplate |
| CN104192967A (en) * | 2014-08-19 | 2014-12-10 | 浙江大学 | Application of Ti3C2 nanosheet in treating high-oxidizability toxic metal ions in water |
| CN104868104A (en) * | 2015-03-27 | 2015-08-26 | 浙江工业大学 | Two-dimensional layered titanium carbide/metal ion composite material and application thereof |
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