CN109052342A - A kind of method of n-methyl-2-pyrrolidone/water binary system ultrasonic wave added removing molybdenum nitride nanometer sheet - Google Patents
A kind of method of n-methyl-2-pyrrolidone/water binary system ultrasonic wave added removing molybdenum nitride nanometer sheet Download PDFInfo
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- CN109052342A CN109052342A CN201810982527.7A CN201810982527A CN109052342A CN 109052342 A CN109052342 A CN 109052342A CN 201810982527 A CN201810982527 A CN 201810982527A CN 109052342 A CN109052342 A CN 109052342A
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- nanometer sheet
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- pyrrolidone
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
- C01B21/062—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with chromium, molybdenum or tungsten
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention discloses a kind of n-methyl-2-pyrrolidone/water binary system ultrasonic wave added removing molybdenum nitride nanometer sheet methods.This method is that after preparing block-like MoN using recrystallization salt template, NMP/H is added in MoN2It is ultrasonic in O binary system, it is then centrifuged for separating, collects supernatant, finally obtain MoN solution.The lamella size for the molybdenum nitride nanometer sheet being stripped out using the method is up to 1 μm, and MoN solution concentration is up to 0.06mg/mL.For the present invention compared with Traditional liquid phase stripping method, the MoN chip size being prepared is big, and yield is high.The method of the present invention is easy to operate, and repeatability is high, which also can be used for the removing of other two-dimensional nano pieces.
Description
Technical field
The present invention relates to molybdenum nitride nanometer sheets to remove field, and in particular to a kind of n-methyl-2-pyrrolidone/water diploid
It is the method for ultrasonic wave added removing molybdenum nitride nanometer sheet.
Background technique
From after successfully isolating graphene, two-dimensional slice material emerges rapidly.The method for obtaining two-dimensional nano piece is mainly divided
It is two kinds, i.e. method and " from bottom to top " method " from top to bottom ".Wherein former approach be primarily referred to as stripping method (such as liquid phase removing
With hot soarfing from etc.), this method operation is fairly simple, and the solvent that currently used liquid phase stripping method uses is mostly N- methyl -2- pyrrole
The single solvents such as pyrrolidone, water and dimethylformamide.The prepared nanometer sheet Mass Distribution come out is uneven, low output；The latter
Mainly self-assembling method, yield is relatively high, and product quality is than more uniform, and prepared by suitable extensive batch, but technique phase
To complexity, solution reaction is required relatively high.
In recent years, MoN has excellent machinery, photoelectricity and magnetic property due to MoN unique structure, in energy storage, urge
Change and there is important application value in semiconductor field.In order to expand the application of MoN nanometer sheet, need to seek a kind of extensive
The reliable method for preparing few layer or single layer MoN nanometer sheet.So far, preparing single layer MoN nanometer sheet is still pendulum at us
Challenge in front, how to prepare high quality monolayer MoN nanometer sheet in a short time using simple experimental facilities is still worth grinding
Study carefully.
Summary of the invention
The purpose of the present invention is to solve currently for production MoN nanometer sheet low output, hardly possible removing there are the problem of with
Defect and a kind of easy to operate, favorable repeatability is provided, prepared lamella is high-quality, and size is big, the high N- methyl -2- of yield
Pyrrolidones/water (NMP/H2O) binary system ultrasonic wave added lift-off technology.
The object of the invention is achieved through the following technical solutions.
A kind of method of n-methyl-2-pyrrolidone/water binary system ultrasonic wave added removing molybdenum nitride nanometer sheet, including with
Lower step:
(1) it disperses molybdenum powder in ethyl alcohol, hydrogen peroxide is then added dropwise and is aoxidized, then pours into sodium-chloride water solution
In, then evaporative crystallization, obtains MoO3@NaCl particle；
(2) by resulting MoO3@NaCl particle is calcined after being ground, then is washed with water, and to remove template salt, obtains block
Shape MoN nanometer sheet；
(3) resulting bulk MoN nanometer sheet will be prepared, ultrasound in n-methyl-2-pyrrolidone/water binary system is added, so
After be centrifugated, collect supernatant, finally obtain MoN nanometer sheet solution.
Further, the concentration of step (1) described sodium-chloride water solution is 30wt%.
Further, the time of step (1) described oxidation is 48 hours.
Further, the temperature of step (1) described evaporative crystallization is 120 DEG C.
Further, the time of step (1) described evaporative crystallization is 6 hours.
Further, step (2) calcining rises to 750 DEG C to be first under argon atmosphere with the heating rate of 5 DEG C/min
Heat preservation 2 hours, then in the argon-mixed (5%NH of ammonia3) under atmosphere, it is small that 650 DEG C of heat preservations 5 are risen to the heating rate of 1 DEG C/min
When.
Further, n-methyl-2-pyrrolidone in n-methyl-2-pyrrolidone/water binary system described in step (3)
Volume ratio with water is 85:15.
Further, the time of step (3) ultrasound is 3 hours.
Further, the condition of step (3) described centrifugation is 2500r/min, 20min.
Further, the concentration of step (3) the MoN nanometer sheet solution is 0.06mg/mL, can generate Tyndall effect,
Illustrate that MoN has dispersibility well.
Further, the MoN chip size is up to 1 μm.
Further, binary system removes principle in step (3) are as follows:
1.NMP and H2O is unlimited miscible in any proportion at any temperature, forms uniform solution.
2. water-soluble on a small quantity can generate a large amount of heat after NMP, produced heat can aggravate the warm-up movement of molecule, and MoN is promoted to receive
The separation of rice piece.In addition, course of dissolution can also generate a large amount of bubble, bubble derives from the O that solution itself dissolves2, CO2Equal gas
Body.And these bubbles also facilitate the separation between MoN lamella.
3.H2H on O molecule can form hydrogen bond with the O in NMP molecule, and the generation of hydrogen bond promotes NMP more closely to adsorb
On MoN nanometer sheet surface.And after forming hydrogen bond, NMP molecular volume is bigger, can effectively prevent the stacking again of MoN nanometer sheet.
Compared with existing stripping means, the present invention has the advantage that
1, the MoN chip size that the method for the present invention is prepared is big, and yield is high.
2, method of the invention is easy to operate, and repeatability is high, is especially advantageous for large scale preparation, has expanded MoN nanometer sheet
Application prospect.In addition the prediction of binary liquid stripping method also can be used for the removing of other two-dimensional nano pieces.
Detailed description of the invention
The SEM figure that Fig. 1 is bulk MoN made from embodiment 1；
Fig. 2 is the SEM figure of MoN nanometer sheet made from embodiment 1；
Fig. 3 is the TEM figure of MoN nanometer sheet made from embodiment 1.
Specific embodiment
Specific implementation of the invention is described further below in conjunction with example and attached drawing, but embodiments of the present invention are not
It is limited to this.
Embodiment 1
It disperses 0.4g molybdenum powder in 20mL ethyl alcohol, 1.4mL hydrogen peroxide is then added dropwise and is aoxidized, fallen after 48 hours
Enter 400ml, in 30wt% sodium chloride (NaCl) aqueous solution, then evaporative crystallization to whole moisture evaporate (6 hours) at 120 DEG C.
By resulting MoO3@NaCl particle is ground, and then first rises to 750 DEG C under argon atmosphere with the heating rate of 5 DEG C/min
Heat preservation 2 hours, then in the argon-mixed (5%NH of ammonia3) under atmosphere, it is small that 650 DEG C of heat preservations 5 are risen to the heating rate of 1 DEG C/min
When calcine, then cleaned with a large amount of deionized waters, to remove template salt, obtain blocky MoN nanometer sheet.The SEM of blocky MoN nanometer sheet
Figure is as shown in Figure 1.It will be seen from figure 1 that products therefrom is laminated structure, surface is clean, and free from admixture generates, and has flexibility.
Resulting 20mg bulk MoN nanometer sheet will be prepared, NMP/H is added2Ultrasound 3 is small in O binary system (85:15, v/v)
When, it is then centrifuged for separating, centrifugal condition 2500r/min, 20min.Supernatant is collected, finally obtaining concentration is 0.06mg/mL
MoN nanometer sheet solution.The SEM figure of MoN nanometer sheet after centrifugation removing is as shown in Figure 2.Figure it is seen that sheet MoN at
Function is stripped down from blocky MoN, and size is up to 1 μm, good dispersion, and yield is high.The TEM of monolithic MoN nanometer sheet schemes such as Fig. 3 institute
Show.From figure 3, it can be seen that MoN nanometer sheet is complete and thin.
Claims (9)
1. a kind of n-methyl-2-pyrrolidone/water binary system ultrasonic wave added removing molybdenum nitride nanometer sheet method, feature exist
In, comprising the following steps:
(1) it disperses molybdenum powder in ethyl alcohol, hydrogen peroxide is then added dropwise and is aoxidized, then pours into sodium-chloride water solution, so
Evaporative crystallization afterwards obtains MoO3@NaCl particle；
(2) by resulting MoO3@NaCl particle is calcined after being ground, then is washed with water, and to remove template salt, obtains blocky MoN
Nanometer sheet；
(3) resulting bulk MoN nanometer sheet will be prepared, ultrasound in n-methyl-2-pyrrolidone/water binary system is added, then from
Heart separation, collects supernatant, finally obtains MoN nanometer sheet solution.
2. the method according to claim 1, wherein the concentration of step (1) described sodium-chloride water solution is
30wt%。
3. the method according to claim 1, wherein the time of step (1) described oxidation is 48 hours.
4. the method according to claim 1, wherein the temperature of step (1) described evaporative crystallization is 120 DEG C.
5. the method according to claim 1, wherein step (2) calcining is first under argon atmosphere, with 5
DEG C/heating rate of min rises to 750 DEG C and keeps the temperature 2 hours, then under the argon-mixed atmosphere of ammonia, with the heating rate of 1 DEG C/min
It rises to 650 DEG C and keeps the temperature 5 hours.
6. the method according to claim 1, wherein n-methyl-2-pyrrolidone/water two described in step (3)
N-methyl-2-pyrrolidone and the volume ratio of water are 85:15 in first system.
7. the method according to claim 1, wherein the time of step (3) ultrasound is 3 hours.
8. the method according to claim 1, wherein the condition of step (3) described centrifugation be 2500 r/min,
20min。
9. the method according to claim 1, wherein the concentration of step (3) the MoN nanometer sheet solution is 0.06
mg/mL。
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Citations (5)
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|---|---|---|---|---|
| WO2011159922A2 (en) * | 2010-06-16 | 2011-12-22 | The Research Foundation Of State University Of New York | Graphene films and methods of making thereof |
| WO2014001519A1 (en) * | 2012-06-28 | 2014-01-03 | The Provost, Fellows, Foundation Scholars, & The Other Members Of Board, Of The College Of The Holy & Undiv. Trinity Of Queen Elizabeth Near Dublin | Atomically thin crystals and films and process for making same |
| CN106672921A (en) * | 2016-12-26 | 2017-05-17 | 华中科技大学 | Preparation method of two-dimensional metal compound material |
| CN107151001A (en) * | 2017-05-18 | 2017-09-12 | 清华-伯克利深圳学院筹备办公室 | A kind of method for preparing high-quality large scale two-dimensional material |
| CN108002374A (en) * | 2017-12-14 | 2018-05-08 | 合肥工业大学 | A kind of ultra-thin two-dimension stratified material nanometer sheet and preparation method thereof |
-
2018
- 2018-08-27 CN CN201810982527.7A patent/CN109052342A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011159922A2 (en) * | 2010-06-16 | 2011-12-22 | The Research Foundation Of State University Of New York | Graphene films and methods of making thereof |
| WO2014001519A1 (en) * | 2012-06-28 | 2014-01-03 | The Provost, Fellows, Foundation Scholars, & The Other Members Of Board, Of The College Of The Holy & Undiv. Trinity Of Queen Elizabeth Near Dublin | Atomically thin crystals and films and process for making same |
| CN106672921A (en) * | 2016-12-26 | 2017-05-17 | 华中科技大学 | Preparation method of two-dimensional metal compound material |
| CN107151001A (en) * | 2017-05-18 | 2017-09-12 | 清华-伯克利深圳学院筹备办公室 | A kind of method for preparing high-quality large scale two-dimensional material |
| CN108002374A (en) * | 2017-12-14 | 2018-05-08 | 合肥工业大学 | A kind of ultra-thin two-dimension stratified material nanometer sheet and preparation method thereof |
Non-Patent Citations (3)
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| KAUSIK MANNA ET AL: ""Toward understanding the efficient exfoliation of layered materials by water-assisted cosolvent liquid-phase exfoliation"", 《CHEMISTRY OF MATERIALS》 * |
| XU XIAO ET AL: ""Salt-Templated synthesis of 2D metallic MoN and other Nitrides"", 《ACS NANO》 * |
| 孙波: ""碳化钼和氮化钼纳米材料的制备与表征"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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Application publication date: 20181221 |