CN109879278A - A kind of preparation method of zero dimension-two dimension hydridization lamination superstructure nano material - Google Patents
A kind of preparation method of zero dimension-two dimension hydridization lamination superstructure nano material Download PDFInfo
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Abstract
The present invention relates to a kind of zero dimension-two dimension hydridization lamination superstructure nano material preparation methods, hydrophily two-dimensional nano piece is surface modified by the method for the present invention by organic ligand molecule, acquisition is dissolved in nonpolar organic polar solvent, modification two-dimensional material with ideal colloid stability, it is uniform that ultrasonic mixing in nonpolar solvent is scattered in prefabricated colloid nanocrystalline particle later, while through solvent volatilization induction lamella stack assembly, instruct nano-crystalline granule in the collaboration ordered fabrication of two-dimensional material piece interlayer using the Van der Waals interaction between ligand molecular, obtain carbon-coated zero dimension-two dimension hydridization lamination superstructure material product.Material inter-layer bonding force prepared by the present invention is strong, compound with regular structure is orderly, electric conductivity is excellent, mechanically and chemically stability is good, and the method for the present invention concise in technology, low energy consumption, securely and reliably, is convenient for large-scale preparation, and is conducive to promote and apply.
Description
Technical field
The invention belongs to field of nanometer material technology, and in particular to be assisted in field of nanometer material technology with nano particle and two-dimensional nano piece
Method with orderly super group dress constructs zero dimension-two-dimension laminate superstructure nano material preparation method.
Background technique
Zero dimension-two-dimension laminate nano material can be with since it combines the good characteristic of two kinds of different dimensions nano materials
So that material is obtained different degrees of promotion in properties such as machinery, optics, electricity and magnetics, receives the extensive concern of people.
Existing zero dimension-two-dimension laminate material preparation method mainly has: 1. simple and mechanical mixing, usually by existing zero
Peacekeeping two-dimension nano materials carry out mechanical mixture by way of simple ultrasound or stirring.The disadvantage is that: it is easy to reunite, structurally ordered
Property is poor, not easy to control etc..2. growth in situ usually grows zero dimensional nanometer materials in two-dimension nano materials surface in situ, still
It is uneven that there are particles, and the disadvantage low in two-dimensional material surface coverage.3. layer by layer deposition method, by chemical vapor deposition,
The modes such as physical vapour deposition (PVD) and electro-deposition obtain zero dimension-two dimension hybrid material, and the disadvantage of sedimentation is time-consuming mistake
It is long, need expensive instrument, it is difficult to produce in batches.4. layer assembly utilizes parents' surfactant, polymerization macromolecule table
Face modification, electrostatic attraction etc. obtain various zero dimensions-two dimension hybrid nano-material by way of LBL self-assembly.
The disadvantages of this method mainly has: localized clusters, and lack of materials in the control of nanoscale, tie between each other by zero dimension-two-dimensional material
It is weak with joint efforts, the separation of zero dimension and two-dimension nano materials is easily caused, so that the materials'use service life is deteriorated, is unfavorable for further reality
Using.
Therefore, develop the labyrinth nano material that effective method carrys out preparation structure high-sequential, no matter
All there is very important theoretical and realistic meaning in basic scientific research or in technical application.
Summary of the invention
It is effective the purpose of the present invention is lacking for existing method to zero dimension-two-dimension laminate superstructure material fine structure
The problem of control, provides a kind of side for cooperateing with orderly super group dress with a two-dimensional nano piece using molecule extension induction nano-crystalline granule
Method prepares the superstructure material with high-sequential laminated construction.This method have it is easy to operate, easily controllable, can largely give birth to
The advantages that production；And the excellent properties such as this superstructure material has compound with regular structure, order is good, is firmly combined.It can be used as function
Material is applied to multiple technical fields such as energy stores and conversion, environmental protection and sea water desalination.
The present invention proposes a kind of preparation method of zero dimension-two dimension hydridization lamination superstructure material, to be commercialized two-dimensional nano
Material (graphene oxide, metal alkene etc.) is raw material, prepares modified two-dimension nano materials through ligand exchange first, then with zero
The uniformly mixing of nanocrystalline colloid ultrasound is tieed up, zero dimension-two dimension hydridization lamination superstructure material is made by solvent volatilization self assembly.Tool
Steps are as follows for body:
(1) preparation of modified two-dimension nano materials dispersion liquid
Two-dimension nano materials are added in nonpolar solvent, the mixture of the two-dimension nano materials is obtained, then to the mixing
Organic amine is added in object, is ultrasonically treated by 1 ~ 200min, obtains dispersion liquid I；Organic acid is added into dispersion liquid I, surpasses again
1 ~ 200min of sonication obtains dispersion liquid II；After anti-solvent is added into dispersion liquid II, centrifugation discards supernatant liquid, lower sediment
Object is modified two-dimension nano materials；Disperse sediment in the two-dimensional nano that the modification is arrived in nonpolar solvent
Material dispersion liquid；
(2) preparation of colloidal nanoparticles dispersion liquid
With the metal compound of the metallic compound of oleic acid, the metallic compound of oleyl amine, the metallic compound of carbonyl or acetylacetone,2,4-pentanedione
Any in object is presoma, and using oleic acid or oleyl amine as ligand molecular, reaction dissolvent is added, and obtains height using high temperature pyrolytic cracking (HTP)
Uniform dispersed nano particle, nano grain surface is coated by organic ligand molecule (oleic acid/oleyl amine), by above-mentioned nanometer
Grain is dissolved in nonpolar solvent, forms stable colloidal nanoparticles dispersion liquid III；
(3) zero dimension-two dimension hydridization lamination superstructure material preparation
By colloidal nanoparticles dispersion liquid III made from modified two-dimension nano materials dispersion liquid made from step (1) and step (2)
It mixes, zero dimension-two-dimension laminate superstructure that ligand is crosslinked is obtained by self assembly of volatilizing after ultrasonic treatment；By the superstructure with
The heating rate of 0.5-50 DEG C/min (N under an inert atmosphere2/ Ar) heat treatment, heat treatment temperature is 100 ~ 800 DEG C, and institute is made
The zero dimension stated-two dimension hydridization lamination superstructure nano material.
In the present invention, in step (1), the mass ratio of the two-dimension nano materials and nonpolar solvent is 1:1 ~ 1:100；Institute
The volume ratio for stating organic amine and nonpolar solvent is 1:1 ~ 1:100；The volume ratio of the organic amine and organic acid is 1:0.1 ~ 1:
10；Volume ratio 1:0.5 ~ 1:10 of the nonpolar solvent and polar solvent.
In the present invention, two-dimension nano materials as described in step (1) are graphene oxide, metal alkene (MXenes), vulcanization
Molybdenum, carbonitride (C3N4), boron nitride, one or more of boron alkene or aluminium oxide.
In the present invention, nonpolar solvent as described in step (1) be n-hexane, toluene, chloroform, hexamethylene carbon tetrachloride,
One or more of methylene chloride, octane, bromoethane, carbon disulfide, tetrachloro-ethylene or tetrahydrofuran.
In the present invention, organic amine as described in step (1) be oleyl amine, 20 amine, cetylamine, lauryl amine, decyl amine, octylame,
One or more of hexylamine or butylamine.
In the present invention, organic acid as described in step (1) be oleic acid, 20 acid, hexadecylic acid, lauric acid/dodecanoic acid, capric acid, octanoic acid,
One or more of caproic acid or butyric acid.
In the present invention, anti-solvent as described in step (1) be one of toluene, acetone, ethyl alcohol, methanol or isopropanol or
It is several.
In the present invention, dispersed nano particle described in step (2) is colloid Fe3O4、MnO、CoO、NiO、TiO、FeS、
MnS、CoS、CuS、SnS、ZnS、FePt、NiPt、FePd、NiPd、Fe、Co、Ni、Pt、Pd、Au、Ag、Cu、Sn、Bi、PbSe、
PbS、CdSe、CdTe、NaYF4Or LaF3It is one or more of nanocrystalline.
In the present invention, the reaction temperature of pyrosol pyrolysismethod described in step (2) is 180 ~ 350 DEG C, and the reaction time is
0.1 ~ 12 hour.
In the present invention, reaction dissolvent described in step (2) be one of octadecylene, octyl ether, hexadecylene or icosa alkene or
It is several.
After the present invention is implemented by adopting the above technical scheme, following effect is mainly generated:
1. the processes such as collaboration assembling, in-situ carburization that the method for the present invention is induced using ligand surface modification, molecule, simple process,
It is easy to operate, it is conducive to large-scale production, it is easy to promote and utilize；
2. the method for the present invention is easy to regulate and control, can be realized by simply changing the allotment of assembling unit to component and structure
Control；Therefore, the method for the present invention can be widely applied to the preparation of periodical high-sequential composite material；
3. the method for the present invention directlys adopt commercialized two-dimensional material, large-scale production easy to accomplish；
4. the zero dimension that the method for the present invention is prepared-two dimension hydridization lamination superstructure material, due to heat treatment process can make it is organic
Ligand molecular in-situ carburization, so that zero-dimension nano particle and two-dimension nano materials are combined in a manner of carbon-to-carbon covalent bond.This
Local mechanical stability not only can be enhanced, it is also ensured that whole flexibility.It can be with relative to simple mechanical mixture
The transfer for preferably realizing two-dimensional material interlayer electronics easily facilitates zero dimension-two dimension hydridization lamination superstructure material and realizes function
On application；
5. the zero dimension that the present invention prepares-two dimension hydridization lamination superstructure material, the structure for having periodical high-sequential is special
Point.This is not only convenient for that the structure change that material generates in application process is observed and tested, also help to material into
Row model construction further theoretically illustrates that material realizes the process and dynamic change of its function.And then targetedly to material
Material is promoted and applied.
It invention can be widely used in the preparation of zero dimension in nano material-two dimension hydridization lamination superstructure material, using this hair
The zero dimension that bright method is prepared-two dimension hydridization lamination superstructure material can be applied to energy stores and conversion, sea water desalination and ring
The fields such as border protection.
Detailed description of the invention
Fig. 1 is the photo in kind after the modified graphene oxide material being dispersed in chloroform in embodiment 1 is placed 7 days；
Fig. 2 is the Fe that embodiment 1 is prepared3O4Nanocrystalline-section graphene hydridization lamination superstructure scanning of materials Electronic Speculum (SEM)
Figure；
Fig. 3 is the Fe that embodiment 1 is prepared3O4Nanocrystalline-section graphene hydridization lamination superstructure scanning of materials Electronic Speculum (SEM)
The enlarged drawing of figure；
Fig. 4 is the Fe that embodiment 1 is prepared3O4Nanocrystalline-graphene hydridization lamination superstructure material SEM front elevation.
Specific embodiment
With reference to embodiment, technical solution of the present invention is described further.
Embodiment 1:
A kind of preparation method of zero dimension-two dimension hydridization lamination superstructure nano material, the specific steps are as follows:
A) preparation of modified two-dimension nano materials dispersion liquid
20 mg graphene oxides are added in 7 g n-hexanes and obtain the mixture of graphene oxide and n-hexane, then to this
2 mL oleyl amines are added in mixture, are ultrasonically treated to obtain dispersion liquid I by 20 min.Further, 2 mL are added into dispersion liquid I
Oleic acid obtains dispersion liquid II again by 5 min of ultrasonic treatment.Further, 30 mL ethyl alcohol are added into dispersion liquid II, are centrifuged
Liquid is discarded supernatant, lower sediment thing is modified graphene oxide material.Further, 10 mL chloroforms are added, just obtain modified two
Dimension nano material dispersion liquid；
B) preparation of colloidal nanoparticles dispersion liquid
18 g iron oleates and 4.3 g oleic acid and 90 g octadecene solvents.Under stirring condition, in 120 DEG C of vacuum outgas
After one hour, 320 DEG C are heated under the protection of nitrogen atmosphere, and keep the temperature 1h. at this temperature.Using high temperature pyrolysis
Method obtains highly homogeneous monodisperse Fe3O4Nano particle, gained nano grain surface are received by there is oleic acid ligand cladding by above-mentioned
Rice grain is dissolved in chloroform, and forming concentration is the stable colloidal nanoparticles dispersion liquid III of 40 mg/mL；
c) Fe3O4The preparation of nanocrystalline-graphene hydridization lamination superstructure material
By gained Fe in gained modified graphene oxide dispersion liquid II in 10 mL step a) and 30 mL step b)3O4Nanocrystalline point
Dispersion liquid III mixes, and obtains the Fe that ligand is crosslinked by solvent volatilization self assembly after ultrasonic treatment3O4Nanocrystalline-graphene oxide is folded
Layer superstructure.Further, the Fe obtained ligand crosslinking ligand being crosslinked3O4Nanocrystalline-graphene lamination superstructure with 3 DEG C/
The heating rate of min is heat-treated (temperature is 500 DEG C) under an inert atmosphere, and Fe is made3O4Nanocrystalline-graphene hydridization lamination is super
Structure；
Selection is dispersed in chloroform solvent after being modified to commercialization graphene oxide using preparation process described in embodiment 1,
There is not apparent noted phase separation phenomena in discovery (as shown in Figure 1) after 7 days stand, and it is very outstanding to illustrate that the dispersion liquid has
Colloidal stability.To the Fe obtained using preparation process described in embodiment 13O4Nanocrystalline-graphene oxide hydridization lamination superstructure
Material is scanned Electronic Speculum (SEM) observation (Fig. 2-4), wherein Fig. 2, and 3 be SEM sectional view, and Fig. 3 is the enlarged drawing of Fig. 2, and Fig. 4 is
SEM front elevation.
From test result analysis it is found that the Fe that the preparation process as described in embodiment 1 obtains3O4Nanocrystalline-graphene hydridization is folded
Fe in layer superstructure material3O4Nano particle it is very regular be embedded into graphene oxide interlayer, it is extremely effective to prevent oxidation
The secondary stacking of graphene.Meanwhile Fe3O4The nano particle arrangement close and orderly in interlayer, is more conducive between nano particle
Being cross-linked with each other in high temperature cabonization.In addition, can obviously find out from test result, it is used for using this method is resulting
The nano particles of lamination superstructure preparation are extremely uniform.Due to the interlamellar spacing of graphene oxide and the ruler of interlayer nano particle
Very little size and uniform level are closely related.Therefore, it can be realized by the adjustment to interlayer nanoparticle size from nanoscale
On the interfloor distance of graphene oxide is regulated and controled.And then can deduce, it by the method for the invention can be by by certain size
Uniform nano particle is embedded in certain nanometer of two-dimensional material, to realize the interlayer for regulating and controlling two-dimensional material on nanoscale
Away from obtaining modularization assembling various dimensions construction unit, this is that other methods are difficult to realize.
Embodiment 2:
A kind of preparation method of zero dimension-two dimension hydridization lamination superstructure nano material, with embodiment 1, in which:
The a) in step, and the mass ratio of graphene oxide and n-hexane is 1:1, and the volume ratio of the oleyl amine and n-hexane is 1:1, oil
The volume ratio of amine and oleic acid is 1:0.1, n-hexane and ethyl alcohol volume ratio 1:0.5；
The b) in step, and high temperature pyrolysis reaction temperature is 180 DEG C, reaction time 0.1h；The c) in step, and heating rate is 0.5 DEG C/
Min, heat treatment temperature are 100 DEG C.
Embodiment 3:
A kind of preparation method of zero dimension-two dimension hydridization lamination superstructure nano material, with embodiment 1, in which:
The a) in step, and the mass ratio of graphene oxide and n-hexane is 1:100, and the volume ratio of the oleyl amine and n-hexane is 1:
100, the volume ratio of oleyl amine and oleic acid is 1:10, n-hexane and ethyl alcohol volume ratio 1:10；
The b) in step, and high temperature pyrolysis reaction temperature is 350 DEG C, reaction time 12h；；
The c) in step, and heating rate is 50 DEG C/min, and heat treatment temperature is 800 DEG C.
Embodiment 4:
A kind of preparation method of zero dimension-two dimension hydridization lamination superstructure nano material, with embodiment 1, in which:
The b) in step, obtains highly homogeneous monodisperse Co nano particle using high temperature pyrolytic cracking (HTP).By the positive trioctylphosphine oxide (TOPO) of 0.1g
(TOPO, 0.15ml oleic acid are dissolved in 15mL o-dichlorohenzene (DCB), and stirring is warming up to 180 DEG C in a nitrogen atmosphere, take 0.54g
Carbonyl cobalt (Co2(CO)8) be dissolved in glove box in 3mL DCB, it is injected into syringe in the DCB and oleic acid solutions of heat, instead
20 minutes should be kept the temperature.Monodisperse Co nano particle is made, the concentration of colloidal nanoparticles dispersion liquid is 20 mg/mL；
C) in step, takes the nanocrystalline dispersion liquid of Co obtained in 10 mL modified graphene oxide dispersion liquids II and 100mL step b)
Ⅲ.Heat treatment temperature is 350 DEG C.
Embodiment 5:
A kind of preparation method of zero dimension-two dimension hydridization lamination superstructure nano material, with embodiment 1, in which:
The b) in step, and the highly homogeneous monodispersed Cu S nano particle obtained using high temperature pyrolytic cracking (HTP) takes 3.18g copper oleate,
It is dissolved in the in the mixed solvent of 50 mL oleyl amines and 50 mL lauryl mercaptans at room temperature, is then warming up to 230 DEG C in a nitrogen atmosphere,
Heat preservation 20min(yellow becomes dark-brown), it is cooled to room temperature, monodispersed Cu S nano particle is made.
C) in step, takes CuS obtained in 10 mL modified graphene oxide dispersion liquids II and 100mL step b) nanocrystalline
Dispersion liquid III.Heat treatment temperature is 300 DEG C.
Embodiment 6:
A kind of preparation method of zero dimension-two dimension hydridization lamination superstructure nano material, with embodiment 1, in which:
The b) in step, the highly homogeneous monodisperse CoFe obtained using high temperature pyrolytic cracking (HTP)2O4Nano particle, by 1.5 g acetyl
Acetone iron, 0.56 g acetylacetone cobalt, 1.2 g enuatrols, 8 mL oleic acid and 20 mL benzyl oxides mix at room temperature.So
290 DEG C are warming up under nitrogen atmosphere afterwards, keeps the temperature 1h.The concentration of colloidal nanoparticles dispersion liquid is 20 mg/mL；
C) in step, takes CoFe obtained in 10 mL modified graphene oxide dispersion liquids II and 100mL step b)2O4It is nanocrystalline
Dispersion liquid III.Heat treatment temperature is 450 DEG C.
Claims (10)
1. a kind of zero dimension-two dimension hydridization lamination superstructure nano material preparation method, it is characterised in that use nano particle and two
Dimension nanometer sheet cooperates with method preparation zero dimension-two dimension hydridization lamination superstructure nano material of orderly super group dress, the specific steps are as follows:
(1) preparation of modified two-dimension nano materials dispersion liquid
Two-dimension nano materials are added in nonpolar solvent, the mixture of two-dimension nano materials is obtained, then to the mixture
Middle addition organic amine is ultrasonically treated by 1 ~ 200min, obtains dispersion liquid I；Organic acid is added into dispersion liquid I, it is ultrasonic again
1 ~ 200min is handled, dispersion liquid II is obtained；After anti-solvent is added into dispersion liquid II, centrifugation discards supernatant liquid, lower sediment thing
As modified two-dimension nano materials；Disperse sediment in the two-dimensional nano material that the modification is arrived in nonpolar solvent
Expect dispersion liquid；
(2) preparation of colloidal nanoparticles dispersion liquid
With the metal compound of the metallic compound of oleic acid, the metallic compound of oleyl amine, the metallic compound of carbonyl or acetylacetone,2,4-pentanedione
Any in object is presoma, using oleic acid or oleyl amine as ligand molecular, reaction dissolvent is added, prepares single point by high temperature pyrolytic cracking (HTP)
Nano particle is dissipated, nano grain surface is coated by organic ligand molecule (oleic acid/oleyl amine), and the nano particle is dissolved in non-pole
In property solvent, stable colloidal nanoparticles dispersion liquid III is formed；
(3) zero dimension-two dimension hydridization lamination superstructure material preparation
By colloidal nanoparticles dispersion liquid III made from modified two-dimension nano materials dispersion liquid made from step (1) and step (2)
It mixes, zero dimension-two-dimension laminate superstructure that ligand is crosslinked is obtained by self assembly of volatilizing after ultrasonic treatment；By the superstructure with
The heating rate of 0.5-50 DEG C/min (N under an inert atmosphere2/ Ar) heat treatment, heat treatment temperature is 100 ~ 800 DEG C, and institute is made
The zero dimension stated-two dimension hydridization lamination superstructure nano material.
2. a kind of zero dimension according to claim 1-two dimension hydridization lamination superstructure material preparation method, feature exist
In in step (1), the mass ratio of the two-dimension nano materials and nonpolar solvent is 1:1 ~ 1:100；The organic amine and non-pole
Property solvent volume ratio be 1:1 ~ 1:100；The volume ratio of the organic amine and organic acid is 1:0.1 ~ 1:10；The nonpolarity is molten
Volume ratio 1:0.5 ~ 1:10 of agent and polar solvent.
3. a kind of zero dimension according to claim 1-two dimension hydridization lamination superstructure material preparation method, feature exist
In two-dimension nano materials as described in step (1) are graphene oxide, metal alkene (MXenes), molybdenum sulfide, carbonitride (C3N4),
One or more of boron nitride, boron alkene or aluminium oxide.
4. a kind of zero dimension according to claim 1-two dimension hydridization lamination superstructure material preparation method, feature exist
In, nonpolar solvent as described in step (1) be n-hexane, toluene, chloroform, hexamethylene carbon tetrachloride, methylene chloride, octane,
One or more of bromoethane, carbon disulfide, tetrachloro-ethylene or tetrahydrofuran.
5. a kind of zero dimension according to claim 1-two dimension hydridization lamination superstructure material preparation method, feature exist
In organic amine as described in step (1) is in oleyl amine, 20 amine, cetylamine, lauryl amine, decyl amine, octylame, hexylamine or butylamine
It is one or more of.
6. a kind of zero dimension according to claim 1-two dimension hydridization lamination superstructure material preparation method, feature exist
In organic acid as described in step (1) is in oleic acid, 20 acid, hexadecylic acid, lauric acid/dodecanoic acid, capric acid, octanoic acid, caproic acid or butyric acid
It is one or more of.
7. a kind of zero dimension according to claim 1-two dimension hydridization lamination superstructure material preparation method, feature exist
In anti-solvent as described in step (1) is one or more of toluene, acetone, ethyl alcohol, methanol or isopropanol.
8. a kind of zero dimension according to claim 1-two dimension hydridization lamination superstructure material preparation method, feature exist
In dispersed nano particle described in step (2) is colloid Fe3O4、MnO、CoO、NiO、TiO、FeS、MnS、CoS、CuS、
SnS、ZnS、FePt、NiPt、FePd、NiPd、Fe、Co、Ni、Pt、Pd、Au、Ag、Cu、Sn、Bi、PbSe、PbS、CdSe、CdTe、
NaYF4Or LaF3It is one or more of nanocrystalline.
9. a kind of zero dimension according to claim 1-two dimension hydridization lamination superstructure material preparation method, feature exist
In the reaction temperature of pyrosol pyrolysismethod described in step (2) is 180 ~ 350 DEG C, and the reaction time is 0.1 ~ 12 hour.
10. a kind of zero dimension according to claim 1-two dimension hydridization lamination superstructure material preparation method, feature exist
In reaction dissolvent described in step (2) is one or more of octadecylene, octyl ether, hexadecylene or icosa alkene.
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| CN113979481B (en) * | 2021-11-09 | 2023-09-05 | 复旦大学 | Preparation method of large-size two-dimensional material |
| CN115058128A (en) * | 2022-06-06 | 2022-09-16 | 江苏大学 | h-BN nano hybrid material and preparation method and application thereof |
| CN115058128B (en) * | 2022-06-06 | 2023-11-10 | 江苏大学 | h-BN nano hybrid material and preparation method and application thereof |
| CN114933297A (en) * | 2022-06-14 | 2022-08-23 | 河南农业大学 | Preparation method of nanocrystalline/carbon nano tube composite super microsphere |
| CN114933297B (en) * | 2022-06-14 | 2023-08-18 | 河南农业大学 | Preparation method of nanocrystalline/carbon nanotube composite super microsphere |
| CN115433464A (en) * | 2022-08-31 | 2022-12-06 | 上海旦元新材料科技有限公司 | Preparation method of interconnected non-close-packed binary superstructure |
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