CN105271231A - Preparation method for two-dimensional nano Ti3C2 sheet - Google Patents

Preparation method for two-dimensional nano Ti3C2 sheet Download PDF

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CN105271231A
CN105271231A CN201510712851.3A CN201510712851A CN105271231A CN 105271231 A CN105271231 A CN 105271231A CN 201510712851 A CN201510712851 A CN 201510712851A CN 105271231 A CN105271231 A CN 105271231A
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CN105271231B (en
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许剑光
姚为
罗驹华
顾大国
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Yangcheng Institute of Technology
Yancheng Institute of Technology
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Abstract

The invention discloses a preparation method for a two-dimensional nano Ti3C2 sheet. The two-dimensional nano Ti3C2 sheet is prepared from Ti3MC2 (M=Si, Al) powder by using a basic hydrothermal synthesis method. The method comprises the following steps: dissolving the superfine Ti3MC2 (M=Si, Al) powder into a basic hydroxide water solution to ultrasonically prepare a suspension; performing hydrothermal treatment to obtain a muddy precipitate; washing, ultrasonically treating, separating and freeze-drying the muddy precipitate to obtain a product. The source of the materials adopted in the preparation method is simple, the prepared Ti3C2 is of a two-dimensional sheet-like nano structure, and is non-corrosive, and high in dispersity, the specific surface area reaches 128.4m<2>/g, and the conversion rate of the product is high.

Description

A kind of two-dimensional nano Ti 3c 2the preparation method of sheet
Technical field
The present invention relates to technical field of nanometer material preparation, be specifically related to a kind of two-dimensional nano Ti 3c 2the preparation method of sheet.
Background technology
Two-dimensional nano Ti 3c 2it is a kind of material the most common in novel class Graphene two-dimension nano materials MXenes family.MXenes two-dimensional material passes through etching MAX compound (as Ti by YuryGogotsi and the MichaelBarsoum seminar of Univ Drexel of the U.S. in 2011 3alC 2deng) obtain first.With Ti 3c 2for the MXenes two-dimensional material of representative has excellent electrical and thermal conductivity, good chemical stability and electrochemical activity, all show good application potential in fields such as lithium ion battery, ultracapacitor, biosensor and gas detection.
Current preparation Ti 3c 2the method that only has be, adopt hydrofluoric acid solution soak Ti 3alC 2powder more than 24 hours, etches away Ti 3alC 2in Al atom, then through the process such as ultrasonic, ion insertion, cleaning, obtain two-dimensional nano Ti 3c 2sheet, as Chinese patent CN104496461A and CN104016345A.Owing to employing the hydrofluoric acid of highly corrosive in preparation process, final product easily adhering to hydrogen fluoride molecule, making Ti when applying 3c 2there is strong corrodibility, limit two-dimensional nano Ti 3c 2the practicality of sheet.Therefore, be necessary to explore the synthetic route novel easy, environmental hazard is little to obtain non-corrosive two-dimensional nano Ti 3c 2sheet.
Summary of the invention
Goal of the invention: for two-dimensional nano Ti in prior art 3c 2preparation method uses the not environmentally problem caused by highly corrosive hydrofluoric acid, the invention provides a kind of environmental protection controlled synthesis polymolecularity two-dimensional nano Ti 3c 2the method of sheet, the Ti that the method is obtained 3c 2product is that two-dimensional nano sheet, non-corrosiveness, good dispersity, specific surface area are large.
Technical scheme: for achieving the above object, the present invention by the following technical solutions:
A kind of two-dimensional nano Ti 3c 2the preparation method of sheet, this preparation method adopts alkaline water thermal synthesis method by Ti 3mC 2powder preparation becomes two-dimensional nano Ti 3c 2sheet, wherein M is Si or Al.
This preparation method comprises the following steps:
(1) Ti is prepared 3mC 2ultrafine powder;
(2) the alkaline hydrated oxide aqueous solution is prepared;
(3) ultrafine powder obtained in step (1) is added in the alkaline hydrated oxide aqueous solution that step (2) prepares, obtain the first mixing solutions, and the first mixing solutions is prepared into suspension;
(4) suspension that step (3) is obtained 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 Ti 3c 2sheet.
Ultrafine powder in described step (1) is with Ti 3mC 2powder is raw material, take Stainless Steel Ball as ball-milling medium, and ball material mass ratio is 5:1, puts into ball grinder, with the rotating speed ball milling 3 hours of 300r/min on planetary ball mill.
Described step (2) neutral and alkali hydroxide aqueous solution adopt deionized water dissolving potassium hydroxide or sodium hydroxide formulated, concentration is 0.5-4mol/L.
Preferably, described step (2) neutral and alkali hydroxide aqueous solution adopts deionized water dissolving potassium hydroxide formulated, and concentration is 1mol/L.
The mass body volume concentrations of the first mixing solutions in described step (3) is that every 30mL alkaline hydrated oxide aqueous solution adds 1g ultrafine powder.
The first mixing solutions in described step (3) ultrasonic 1 hour at ambient temperature, is prepared into suspension.
Sludge in described step (4) is that the suspension obtained in step (3) is put into water heating kettle, is placed in baking oven and is heated to 240 DEG C and is incubated 24 hours, poured out by supernatant liquid after cooling, namely obtain sludge, for subsequent use.
The method preparing colloidal solution in described step (5) pours the sludge obtained in step (4) into beaker, first uses deionized water wash twice, then with absolute ethanol washing once; Add after washing and be mixed with the second mixing solutions liquid with the deionized water of alkaline hydrated oxide aqueous solution volume equivalent that uses in step (3), then by the second mixing solutions ultrasonic 3 hours at ambient temperature, sediment separate out, namely obtained colloidal solution.
Two-dimensional nano Ti in described step (6) 3c 2sheet is that the colloidal solution of gained in step (5) is put into freezer compartment of refrigerator after freezing 24 hours, then puts into Freeze Drying Equipment vacuum-freeze-dry and be prepared from.
Beneficial effect: compared with prior art, the present invention has following advantage:
(1) this nano material is prepared from Ti 3siC 2, Ti 3alC 2start etc. simple inorganics, source is simple; Use the alkaline hydrated oxide aqueous solution to replace traditional hydrofluoric acid to etch in preparation method, corrodibility reduces, and then can obtain the lamella Ti with nanoscale through stripping, freeze-drying 3c 2material.
(2) product that prepared by the present invention is the two-dimensional nano sheet of pattern rule, non-corrosiveness, good dispersity, specific surface area can reach 128.4m 2/ g.
(3) conversion rate of products of the present invention is high, and transformation efficiency can reach more than 75%.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described, and the description of specific embodiment is only example in essence, instead of intend to limit content disclosed by the invention and application thereof or use.
Embodiment 1
(1) with Ti 3siC 2powder is raw material, take Stainless Steel Ball as ball-milling medium, and ball material mass ratio is 5:1, puts into ball grinder, according to the rotating speed ball milling 3 hours of 300r/min on planetary ball mill, obtains Ti 3siC 2ultrafine powder;
(2) fully stir with deionized water under room temperature potassium hydroxide is dissolved, obtain potassium hydroxide aqueous solution, concentration is 1mol/L;
(3) Ti in step (1) is got 3siC 2the potassium hydroxide aqueous solution that ultrafine powder adds step (2) obtained is mixed to get the first mixing solutions, and wherein every 30mL potassium hydroxide aqueous solution adds 1gTi 3siC 2ultrafine powder; Again by the first mixing solutions at room temperature ultrasonic 1 hour, obtain muddy suspension;
(4) suspension in step (3) is got, pour in polytetrafluoroethylliner liner, reinstall in water heating kettle, be placed in baking oven be heated to 240 DEG C and be incubated 24 hours, open reactor after cooling, supernatant liquid in polytetrafluoroethylliner liner is poured out, then takes out the sludge of bottom;
(5) get the sludge in step (4), pour beaker into, first use deionized water wash twice, then with absolute ethanol washing once; Add after washing and prepare the second mixing solutions with the deionized water of potassium hydroxide aqueous solution volume equivalent that uses in step (3), then by the second mixing solutions ultrasonic 3 hours at ambient temperature, sediment separate out, namely obtained navy blue colloidal solution;
(6) colloidal solution got in step (5) puts into freezer compartment of refrigerator after freezing 24 hours, then puts into Freeze Drying Equipment vacuum-freeze-dry, both obtains two-dimensional nano Ti 3c 2sheet.
Performance perameter: the two-dimensional nano Ti of acquisition 3c 2sheet is pure Ti through XRD test 3c 2phase, calculating by weight transformation efficiency is 91.5%, and specific surface area is 122.9m through BET test 2/ g.
Embodiment 2
(1) with Ti 3siC 2powder is raw material, take Stainless Steel Ball as ball-milling medium, and ball material mass ratio is 5:1, puts into ball grinder, according to the rotating speed ball milling 3 hours of 300r/min on planetary ball mill, obtains Ti 3siC 2ultrafine powder;
(2) fully stir with deionized water under room temperature potassium hydroxide is dissolved, obtain potassium hydroxide aqueous solution, concentration is 0.5mol/L;
(3) Ti in step (1) is got 3siC 2the potassium hydroxide aqueous solution that ultrafine powder adds step (2) obtained is mixed to get the first mixing solutions, and wherein every 30mL potassium hydroxide aqueous solution adds 1gTi 3siC 2ultrafine powder; Again by the first mixing solutions at room temperature ultrasonic 1 hour, obtain muddy suspension;
(4) suspension in step (3) is got, pour in polytetrafluoroethylliner liner, reinstall in water heating kettle, be placed in baking oven be heated to 240 DEG C and be incubated 24 hours, open reactor after cooling, supernatant liquid in polytetrafluoroethylliner liner is poured out, then takes out the sludge of bottom;
(5) get the sludge in step (4), pour beaker into, first use deionized water wash twice, then with absolute ethanol washing once; The deionized water adding the potassium hydroxide aqueous solution volume equivalent used with step (3) after washing prepares the second mixing solutions, then by the second mixing solutions ultrasonic 3 hours at ambient temperature, sediment separate out, i.e. obtained navy blue colloidal solution;
(6) colloidal solution got in step (5) puts into freezer compartment of refrigerator after freezing 24 hours, then puts into Freeze Drying Equipment vacuum-freeze-dry, both obtains two-dimensional nano Ti 3c 2sheet.
Performance perameter: the two-dimensional nano Ti of acquisition 3c 2sheet is pure Ti through XRD test 3c 2phase, calculating by weight transformation efficiency is 85.2%, and specific surface area is 100.7m through BET test 2/ g.
Embodiment 3
(1) with Ti 3siC 2powder is raw material, take Stainless Steel Ball as ball-milling medium, and ball material mass ratio is 5:1, puts into ball grinder, according to the rotating speed ball milling 3 hours of 300r/min on planetary ball mill, obtains Ti 3siC 2ultrafine powder;
(2) fully stir with deionized water under room temperature potassium hydroxide is dissolved, obtain potassium hydroxide aqueous solution, concentration is 4mol/L;
(3) Ti in step (1) is got 3siC 2the potassium hydroxide aqueous solution that ultrafine powder adds step (2) obtained is mixed to get the first mixing solutions, and wherein every 30mL potassium hydroxide aqueous solution adds 1gTi 3siC 2ultrafine powder; Again by the first mixing solutions at room temperature ultrasonic 1 hour, obtain muddy suspension;
(4) suspension in step (3) is got, pour in polytetrafluoroethylliner liner, reinstall in water heating kettle, be placed in baking oven be heated to 240 DEG C and be incubated 24 hours, open reactor after cooling, supernatant liquid in polytetrafluoroethylliner liner is poured out, then takes out the sludge of bottom;
(5) get the sludge in step (4), pour beaker into, first use deionized water wash twice, then with absolute ethanol washing once; The deionized water adding the potassium hydroxide aqueous solution volume equivalent used with step (3) after washing prepares the second mixing solutions, then by the second mixing solutions ultrasonic 3 hours at ambient temperature, sediment separate out, i.e. obtained navy blue colloidal solution;
(6) colloidal solution got in step (5) puts into freezer compartment of refrigerator after freezing 24 hours, then puts into Freeze Drying Equipment vacuum-freeze-dry, both obtains two-dimensional nano Ti 3c 2sheet.
Performance perameter: the two-dimensional nano Ti of acquisition 3c 2sheet is pure Ti through XRD test 3c 2phase, calculating by weight transformation efficiency is 92.6%, and specific surface area is 128.4m through BET test 2/ g.
Embodiment 4
(1) with Ti 3alC 2powder is raw material, take Stainless Steel Ball as ball-milling medium, and ball material mass ratio is 5:1, puts into ball grinder, according to the rotating speed ball milling 3 hours of 300r/min on planetary ball mill, obtains Ti 3alC 2ultrafine powder;
(2) fully stir with deionized water under room temperature potassium hydroxide is dissolved, obtain potassium hydroxide aqueous solution, concentration is 1mol/L;
(3) Ti in step (1) is got 3alC 2the potassium hydroxide aqueous solution that ultrafine powder adds step (2) obtained is mixed to get the first mixing solutions, and wherein every 30mL potassium hydroxide aqueous solution adds 1gTi 3alC 2ultrafine powder; Again by the first mixing solutions at room temperature ultrasonic 1 hour, obtain muddy suspension;
(4) suspension in step (3) is got, pour in polytetrafluoroethylliner liner, reinstall in water heating kettle, be placed in baking oven be heated to 240 DEG C and be incubated 24 hours, open reactor after cooling, supernatant liquid in polytetrafluoroethylliner liner is poured out, then takes out the sludge of bottom;
(5) get the sludge in step (4), pour beaker into, first use deionized water wash twice, then with absolute ethanol washing once; Add after washing and prepare the second mixing solutions with the deionized water of potassium hydroxide aqueous solution volume equivalent that uses in step (3), then by the second mixing solutions ultrasonic 3 hours at ambient temperature, sediment separate out, namely obtained navy blue colloidal solution;
(6) colloidal solution got in step (5) puts into freezer compartment of refrigerator after freezing 24 hours, then puts into Freeze Drying Equipment vacuum-freeze-dry, both obtains two-dimensional nano Ti 3c 2sheet.
Performance perameter: the two-dimensional nano Ti of acquisition 3c 2sheet is pure Ti through XRD test 3c 2phase, calculating by weight transformation efficiency is 81.6%, and specific surface area is 106.3m through BET test 2/ g.
Embodiment 5
(1) with Ti 3siC 2powder is raw material, take Stainless Steel Ball as ball-milling medium, and ball material mass ratio is 5:1, puts into ball grinder, according to the rotating speed ball milling 3 hours of 300r/min on planetary ball mill, obtains Ti 3siC 2ultrafine powder;
(2) fully stir with deionized water under room temperature sodium hydroxide is dissolved, obtain aqueous sodium hydroxide solution, concentration is 1mol/L;
(3) Ti in step (1) is got 3siC 2the aqueous sodium hydroxide solution that ultrafine powder adds step (2) obtained is mixed to get the first mixing solutions, and wherein every 30mL aqueous sodium hydroxide solution adds 1gTi 3siC 2ultrafine powder; Again by the first mixing solutions at room temperature ultrasonic 1 hour, obtain muddy suspension;
(4) suspension in step (3) is got, pour in polytetrafluoroethylliner liner, reinstall in water heating kettle, be placed in baking oven be heated to 240 DEG C and be incubated 24 hours, open reactor after cooling, supernatant liquid in polytetrafluoroethylliner liner is poured out, then takes out the sludge of bottom;
(5) get the sludge in step (4), pour beaker into, first use deionized water wash twice, then with absolute ethanol washing once; Add after washing and prepare the second mixing solutions with the deionized water of aqueous sodium hydroxide solution volume equivalent that uses in step (3), then by the second mixing solutions ultrasonic 3 hours at ambient temperature, sediment separate out, namely obtained navy blue colloidal solution;
(6) colloidal solution got in step (5) puts into freezer compartment of refrigerator after freezing 24 hours, then puts into Freeze Drying Equipment vacuum-freeze-dry, both obtains two-dimensional nano Ti 3c 2sheet.
Performance perameter: the two-dimensional nano Ti of acquisition 3c 2sheet is purer Ti through XRD test 3c 2phase, calculating by weight transformation efficiency is 75.5%, and specific surface area is 108.5m through BET test 2/ g.
Should be understood that; above embodiment is only optimal way of the present invention; only that illustrated example effect is played to technical conceive of the present invention; can not limit the scope of the invention with this; those skilled in the art are not departing from the spirit and scope of technical solution of the present invention; modify and be equal to replacement, all should drop within protection scope of the present invention.

Claims (10)

1. a two-dimensional nano Ti 3c 2the preparation method of sheet, is characterized in that: described preparation method adopts alkaline water thermal synthesis method by Ti 3mC 2powder preparation becomes two-dimensional nano Ti 3c 2sheet, wherein M is Si or Al.
2. two-dimensional nano Ti according to claim 1 3c 2the preparation method of sheet, is characterized in that: described preparation method specifically comprises the following steps:
(1) Ti is prepared 3mC 2ultrafine powder;
(2) the alkaline hydrated oxide aqueous solution is prepared;
(3) ultrafine powder obtained in step (1) is added in the alkaline hydrated oxide aqueous solution that step (2) prepares, obtain the first mixing solutions, and the first mixing solutions is prepared into suspension;
(4) suspension that step (3) is obtained 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 Ti 3c 2sheet.
3. two-dimensional nano Ti according to claim 2 3c 2the preparation method of sheet, is characterized in that: the ultrafine powder described in step (1) is with Ti 3mC 2powder is raw material, take Stainless Steel Ball as ball-milling medium, and ball material mass ratio is 5:1, puts into ball grinder, with the rotating speed ball milling 3 hours of 300r/min on planetary ball mill.
4. two-dimensional nano Ti according to claim 2 3c 2the preparation method of sheet, is characterized in that: in step (2), the described alkaline hydrated oxide aqueous solution adopt deionized water dissolving potassium hydroxide or sodium hydroxide formulated, concentration is 0.5-4mol/L.
5. two-dimensional nano Ti according to claim 4 3c 2the preparation method of sheet, is characterized in that: in step (2), and the described alkaline hydrated oxide aqueous solution adopts deionized water dissolving potassium hydroxide formulated, and concentration is 1mol/L.
6. two-dimensional nano Ti according to claim 2 3c 2the preparation method of sheet, is characterized in that: the mass body volume concentrations of the first mixing solutions described in step (3) is that every 30mL alkaline hydrated oxide aqueous solution adds 1g ultrafine powder.
7. the two-dimensional nano Ti according to claim 2 or 6 3c 2the preparation method of sheet, is characterized in that: by the first mixing solutions ultrasonic 1 hour at ambient temperature in step (3), be prepared into suspension.
8. two-dimensional nano Ti according to claim 2 3c 2the preparation method of sheet, it is characterized in that, the 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 is heated to 240 DEG C and is incubated 24 hours, after cooling supernatant liquid is poured out, namely obtain sludge.
9. two-dimensional nano Ti according to claim 2 3c 2the preparation method of sheet, is characterized in that, colloidal solution described in step (5) pours the sludge obtained in step (4) into beaker, first uses deionized water wash twice, then with absolute ethanol washing once; Add after washing and be mixed with the second mixing solutions liquid with the deionized water of alkaline hydrated oxide aqueous solution volume equivalent that uses in step (3), then by the second mixing solutions ultrasonic 3 hours at ambient temperature, sediment separate out, namely obtained colloidal solution.
10. preparation method according to claim 2, is characterized in that, the two-dimensional nano Ti described in step (6) 3c 2sheet is that the colloidal solution of gained in step (5) is put into freezer compartment of refrigerator after freezing 24 hours, then puts into Freeze Drying Equipment vacuum-freeze-dry and be prepared from.
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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN105905870A (en) * 2016-04-15 2016-08-31 广东工业大学 Preparation method of metallic oxide two-dimensional nano-material
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
CN106784779A (en) * 2016-12-19 2017-05-31 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
CN110723737A (en) * 2019-10-24 2020-01-24 郑州轻工业学院 Wool ball type Ti3C2Preparation method and application of (MXene) nano material
CN111232981A (en) * 2020-01-17 2020-06-05 北京理工大学 High lithium storage capacity Ti3C2TxMechanochemical preparation method of
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

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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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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

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105905870A (en) * 2016-04-15 2016-08-31 广东工业大学 Preparation method of metallic oxide two-dimensional nano-material
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
CN106784779A (en) * 2016-12-19 2017-05-31 盐城工学院 A kind of preparation method of nano lithium titanate and the preparation method of cell negative electrode material
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
CN110723737A (en) * 2019-10-24 2020-01-24 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
CN111232981A (en) * 2020-01-17 2020-06-05 北京理工大学 High lithium storage capacity Ti3C2TxMechanochemical preparation method of
CN111232981B (en) * 2020-01-17 2020-12-29 北京理工大学 High lithium storage capacity Ti3C2TxMechanochemical preparation method of

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