CN110526293A - A kind of method that easy salt decomposition auxiliary prepares two-dimension nano materials - Google Patents
A kind of method that easy salt decomposition auxiliary prepares two-dimension nano materials Download PDFInfo
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- CN110526293A CN110526293A CN201910865043.9A CN201910865043A CN110526293A CN 110526293 A CN110526293 A CN 110526293A CN 201910865043 A CN201910865043 A CN 201910865043A CN 110526293 A CN110526293 A CN 110526293A
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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
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
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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
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
Abstract
A kind of method that easy salt decomposition auxiliary prepares two-dimension nano materials, belongs to two-dimension nano materials preparation technical field.After stratified material (graphite, molybdenum disulfide etc.) and the easy salt decomposition mixing and ball milling of low temperature, by annealing, pre- intercalation powder is obtained, dispersion liquid is made into, removed by ultrasound or high shear, the two-dimension nano materials less than ten layers can be obtained.The present invention is conducive to crush stratified material and prevents lamella from stacking again, furthermore using easy salt decomposition as removing auxiliary agent, part easily salt decomposition can be inserted into the interlayer of Layering powder, be conducive to shearing removing, the obtained two-dimensional nano piece number of plies is few, nanometer chip size is controllable, and yield is high.This method charge stripping efficiency is high, preparation is simple, has many advantages, such as industrial applications prospect.
Description
Technical field
The invention belongs to two-dimension nano materials preparation technical fields more particularly to liquid phase shearing removing to prepare two-dimensional nano material
The application in material field.
Background technique
Nano material has small size, surface and interface, quantum size, macroscopic quantum tunneling etc. compared to body phase material
Effect, just because of these special properties and rule, nano material has extensively in fields such as optics, magnetics, electronics, biology
Wealthy application prospect.Since two thousand four, Novoselov et al. prepares graphene by micromechanics stripping method, it was demonstrated that two dimension
Nano material can be stabilized at ambient conditions.Everybody traditional cognitive to two-dimension nano materials has been broken in this discovery,
Promote the preparation of more and more researcher's study two-dimensional ultrathin nanometer materials, property and application.For example graphene, transition gold
Belong to sulfide (such as molybdenum disulfide, tungsten disulfide), transition metal oxide (such as molybdenum oxide, titanium oxide), Mxene two-dimensional nano
Material has very big development potentiality in device, energy storage, sensing, catalysis, medicine and other fields, still, it is desirable to realize two-dimensional nano
Material is badly in need of developing a kind of side of preparation high quality nanometer sheet simple, efficient, at low cost in the industrial applications in each field
Method is one of bottleneck for being nowadays badly in need of capturing and present research emphasis and difficult point.
Currently, the common mode for preparing two-dimension nano materials includes that (such as hydrothermal synthesis method is vapor-deposited method from bottom to top
Method, epitaxial growth method), method (such as lithium ion graft process, oxidation-reduction method, electrochemical stripping method, supercritical fluid stripping from top to bottom
From method, liquid phase stripping method).Wherein, method and lithium ion graft process from bottom to top, although preparation product quality is high, yield is high,
Operating environment requirement is harsh, and post-processing is cumbersome, easily introducing impurity, influences properties of product；Redox rule is often accompanied by product
Defect is more, easily causes the problem of environmental pollution；And electrochemical stripping method drives yin-yang in electrolyte solution using electric field action
The intercalation repeatedly of ion, the final two-dimension nano materials for obtaining few layer, the cost is relatively high for this method, it is difficult to realize extensive raw
It produces；In addition, the supercritical fluid stripping method risen in the recent period, although simple process, advantage of lower cost, operating process needs
Higher pressure is kept for a long time, promotes supercritical fluid intercalation stripping, and the safety operation problem of this method becomes industry amplification
Difficult point；In view of productivity and operation cost, liquid phase stripping method is considered as one of the mode that pole is easy to realize industrial production, because
It is easy to operate, efficient for this method, nano material can be prepared without particular surroundings.In liquid phase stripping process, equipment is needed
Enough energy are provided, such as ultrasound, shearing equipment, the Van der Waals force for overcoming stratified material interlayer weaker, also needs selection suitable
Auxiliary agent and solvent up-stripping are dispersed in water, You Jirong for example by natural block raw material or chemically synthesized raw material
In agent, cosolvent or ionic liquid, and suitable auxiliary agent, such as surfactant are selected, salt, metal hydroxides or polymer etc.
Up-stripping improves the yield and dispersion stabilization of nanometer sheet.Although liquid phase stripping method prepares the method layer of two-dimension nano materials
It is not poor out, but yield is relatively low at present, it usually needs pretreatment improves yield, as Microwave Pretreatment, dry ice assist ball milling
Deng generally requiring the additive of special environment or valuableness, cause process costs to increase, be unfavorable for industrialized production.Therefore, it opens
It sends out one kind at normal temperatures and pressures, yield and product quality can be improved, be conducive to industry amplification, the removing of efficient liquid phase
Method is the research hotspot of nowadays field of nano material preparation.
The present invention is using easy salt decomposition as auxiliary agent, under ball milling, the processing of ultrasound/high-shear mixer, with it is simple, efficient,
Economic mode, successfully prepares the high two-dimensional nano piece of surface cleaning, yield.Advantage using easy salt decomposition as auxiliary agent exists
In: (1) play the role of physical grinding, accelerates raw material ball mill grinding process, while preventing lamella from stacking again.(2) easy salt decomposition
It easily decomposes, post-processing is simple, and i.e. separable by high temperature, product quality is high, is not introduced into impurity.(3) easily salt decomposition can be inserted partially
Enter stratified material interlayer, weaken interlayer Van der Waals force, improves removing yield.(4) it is at low cost to compare other auxiliary agents for easy salt decomposition.Together
When, using ball milling, ultrasound or the high-shear mixer of easily scale amplification as peel-off device, improves this method and realize industry
Change manufacturing feasibility.
Summary of the invention
The present invention provides the new method that a kind of easy salt decomposition auxiliary prepares two-dimension nano materials.Using easy salt decomposition as helping
Agent, assist ball milling, by annealing after obtain pre- intercalation powder, by pre- intercalation powder dispersion in a solvent, by ultrasound or
High shear removing, obtained two-dimension nano materials quality is high, defect is few.
The invention discloses a kind of methods that easy salt decomposition auxiliary prepares two-dimension nano materials, including process below and step
It is rapid:
1) it using bulky grain stratified material as raw material, after being mixed in a certain proportion ball milling with easy salt decomposition, is made annealing treatment,
Extra easy salt decomposition is removed while annealing, is increased the Layering powder interlamellar spacing tentatively crushed, is obtained the powder of pre- intercalation；
2) powder for the pre- intercalation that step 1) obtains is made into dispersion liquid, in ultrasound or high-shear mixer, is shelled
Two-dimension nano materials are obtained from processing.
The block stratified material of step 1) includes and is not limited to: various graphite (natural graphite, expanded graphite, crystalline flake graphites
Deng), molybdenum disulfide (natural molybdenum disulfide, synthesis of carbon/molybdenum disulfide) etc..
The easy salt decomposition of step 1), including and be not limited to: labile carbonate, such as: ammonium hydrogen carbonate, ammonium carbonate and urea
Deng；Labile nitrate, oxalates and hydrochloride, the salt in nitrate, oxalates and hydrochloride are the salt of ammonium class, etc..
The bulky grain stratified material of step 1) and the mass ratio of easy salt decomposition are 1:0.1-1:10.
The Ball-milling Time of step 1) is 1-24h, rotational speed of ball-mill 50-350rpm.
The annealing of step 1) carries out under inert gas protection, and minimum annealing temperature is easy salt decomposition initial decomposition
Temperature, highest annealing temperature are 900 DEG C, and heating rate is 2-10 DEG C/min, and anneal 2h.
The pre- intercalation powder of step 2) can be dispersed into different solutions, such as organic solvent, water, cosolvent.
Ultrasonic treatment described in step 2), i.e., the ultrasonic cavitation generated using instruments such as ultrasonic cleaner, probe sonications
Effect is removed, ultrasonic power 200W, splitting time 1-6h.
The processing of high-shear mixer described in step 2) moves narrow gap between rotor using mixer, generate compared with
High local energy-dissipation rate and great shear rate are removed, and revolving speed 300-18000rpm/min, removing are removed
Time 1-6h.
This method is easy to operate, efficient, at low cost, suitable for scale production, is with a wide range of applications.
Detailed description of the invention
It is described further in conjunction with picture for specific embodiments of the present invention；
The TEM figure of the two-dimentional molybdenum disulfide of the removing preparation of Fig. 1 embodiment of the present invention 1；
The TEM figure of the graphene of the removing preparation of Fig. 2 embodiment of the present invention 12；
The AFM figure of the graphene of the removing preparation of Fig. 3 embodiment of the present invention 12；
The conductivity of the graphene of the removing preparation of Fig. 4 embodiment of the present invention 12 is with pressure change curve graph；
Specific embodiment
It is of the invention for ease of understanding, following specific embodiments will be enumerated, is described in further detail, protection model of the invention
Enclosing should include the full content of claim and specific embodiment, but be not limited to this, in the condition without departing substantially from the scope of the invention
Under, various changes that those of ordinary skill in the art are able to carry out.
Embodiment 1
Prepare molybdenum disulfide nano sheet；
The molybdenum disulfide of block is mixed with ammonium hydrogen carbonate with mass ratio 1:2, rotational speed of ball-mill 320rpm, ball milling
6h；
Powder after ball milling is handled by tube annealing, under inert atmosphere protection, with the heating speed of 10 DEG C/min
After degree rises to 200 DEG C, 2h is kept the temperature, the ammonium hydrogen carbonate of non-intercalation is decomposed；
Pre- intercalation powder is dispersed to again in NMP organic solvent, after concentration 30mg/mL, ultrasonic 1h, by suspension from
After the heart, supernatant is taken, obtains molybdenum disulfide nano sheet dispersion liquid.Molybdenum disulfide nano sheet dispersion liquid concentration is 11.1mg/mL, is put down
Equal lateral dimension about 64nm, the number of plies are less than 10 layers, yield 37%.Gained molybdenum disulfide nano sheet pattern, as shown in Figure 1.
Embodiment 2
Embodiment 2 is mixed with 1 difference of example for block molybdenum disulfide with ammonium chloride with mass ratio 1:2, remaining
Process is consistent, after ultrasonic treatment, yield 20%.
Embodiment 3
Embodiment 3 and 1 difference of example are that high-shear mixer removes 2h, revolving speed 8000rpm/min, remaining process
Unanimously, after ultrasonic treatment, yield 30%；
Embodiment 4
Embodiment 4 and 1 difference of example are that the heating rate of annealing is 2 DEG C/min, remaining process is consistent, ultrasound
After processing, yield 29%；
Embodiment 5
Embodiment 5 and 1 difference of example are that the holding temperature of annealing is 900 DEG C, remaining process is consistent, at ultrasound
After reason, yield 10%；
Embodiment 6
Embodiment 6 and 1 difference of example are that the holding temperature of annealing is 60 DEG C, remaining process is consistent, at ultrasound
After reason, yield 25%；
Embodiment 7
Prepare graphene nanometer sheet；
The graphite of block is mixed with ammonium hydrogen carbonate with mass ratio 1:2, ball milling speed 320rpm, ball milling 8h；
Powder after ball milling is handled by tube annealing, under inert atmosphere protection, with the heating speed of 10 DEG C/min
After degree rises to 200 DEG C, 2h is kept the temperature, the ammonium hydrogen carbonate of non-intercalation is decomposed；
Pre- intercalation powder is dispersed to again in NMP organic solvent, after concentration 20mg/mL, ultrasonic 1h, by suspension from
After the heart, supernatant is taken, obtains graphene dispersing solution, concentration 2.6mg/mL, yield 13%.
Embodiment 8
The graphite and ammonium hydrogen carbonate that embodiment 8 and 7 difference of example are block are with mass ratio 1:0.5, remaining process one
It causes, yield 4%.
Embodiment 9
For the graphite and ammonium hydrogen carbonate that embodiment 9 and 7 difference of example are block with mass ratio 1:1, remaining process is consistent,
Yield is 8%.
Embodiment 10
Embodiment 10 and 7 difference of example are ball milling 16h, remaining process is consistent, yield 22%；
Embodiment 11
Embodiment 11 and 7 difference of example be ball milling for 24 hours, remaining process is consistent, yield 30%；
Embodiment 12
Embodiment 12 is that preferably ball milling 16h, ultrasonic 5h, remaining process is consistent, yield 41% with 7 difference of example,
Gained graphene nanometer sheet transverse direction face size concentrates on 0~1.3 μm (being not 0), and the number of plies is at 5~6 layers, as shown in Figure 2,3.
Graphene powder is prepared with high conductance, is 14285S/m, as shown in Figure 4.
Embodiment 13
Embodiment 13 is that preferably ball milling 16h, ultrasonic 6h, remaining process is consistent, yield 40% with 7 difference of example.
Claims (10)
1. a kind of method that easy salt decomposition auxiliary prepares two-dimension nano materials, which is characterized in that including process below and step:
1) it using bulky grain stratified material as raw material, after being mixed in a certain proportion ball milling with easy salt decomposition, is made annealing treatment, is annealed
While remove extra easy salt decomposition, make the Layering powder interlamellar spacing tentatively crushed increase, obtain the powder of pre- intercalation；
2) powder for the pre- intercalation that step 1) obtains is made into dispersion liquid, ultrasound or high-shear mixer in, carry out removing and
Processing obtains two-dimension nano materials.
2. the method that a kind of easy salt decomposition auxiliary described in accordance with the claim 1 prepares two-dimension nano materials, which is characterized in that step
Rapid block stratified material 1) is various graphite (natural graphite, expanded graphite, crystalline flake graphite etc.), molybdenum disulfide (natural two sulphur
Change molybdenum, synthesis of carbon/molybdenum disulfide) etc..
3. the method that a kind of easy salt decomposition auxiliary described in accordance with the claim 1 prepares two-dimension nano materials, which is characterized in that step
Rapid easy salt decomposition 1), for any one or a few in carbonate and labile nitrate, oxalates and hydrochloride.
4. the method that a kind of easy salt decomposition auxiliary described in accordance with the claim 3 prepares two-dimension nano materials, which is characterized in that carbon
Hydrochlorate is selected from ammonium hydrogen carbonate, ammonium carbonate and urea；Salt in nitrate, oxalates and hydrochloride is the salt of ammonium class.
5. the method that a kind of easy salt decomposition auxiliary described in accordance with the claim 1 prepares two-dimension nano materials, big of step 1)
The mass ratio of grain stratified material and easy salt decomposition is 1:0.1-1:10.
6. the method that a kind of easy salt decomposition auxiliary described in accordance with the claim 1 prepares two-dimension nano materials, the ball milling of step 1)
Time is 1-24h, rotational speed of ball-mill 50-350rpm.
7. the method that a kind of easy salt decomposition auxiliary described in accordance with the claim 1 prepares two-dimension nano materials, the annealing of step 1)
Processing, carries out under inert gas protection, and minimum annealing temperature is easy salt decomposition temperature of initial decomposition, and highest annealing temperature is
900 DEG C, heating rate is 2-10 DEG C/min, annealing time 2h.
8. the method that a kind of easy salt decomposition auxiliary described in accordance with the claim 1 prepares two-dimension nano materials, step 2) it is pre-inserted
Layer powder can be dispersed into different solutions, such as organic solvent, water, cosolvent.
9. the method that a kind of easy salt decomposition auxiliary described in accordance with the claim 1 prepares two-dimension nano materials, described in step 2)
Ultrasonic treatment is removed, ultrasonic power using the ultrasound cavitation effect that the instruments such as ultrasonic cleaner, probe sonication generate
200W, splitting time 1-6h.
10. the method that a kind of easy salt decomposition auxiliary described in accordance with the claim 1 prepares two-dimension nano materials, described in step 2)
High-shear mixer processing generates higher local energy-dissipation rate that is, using gap narrow between the dynamic rotor of mixer
And greatly shear rate is removed, and removes revolving speed 300-18000rpm/min, splitting time 1-6h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113526556A (en) * | 2021-07-12 | 2021-10-22 | 济南大学 | Single crystal particle assembled lamella WNb2O8And preparation method and application thereof |
| CN113772732A (en) * | 2021-09-26 | 2021-12-10 | 江南大学 | Method for preparing two-dimensional material nanosheet by DEET stripping |
| GB2603861A (en) * | 2021-02-11 | 2022-08-17 | Cami Consultancy Ltd | Graphene Production Method |
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| CN113772732B (en) * | 2021-09-26 | 2022-05-06 | 江南大学 | Method for preparing two-dimensional material nanosheet by DEET stripping |
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