CN110255517A - Inorganic organic intercalation superlattice film of large area flexible and preparation method thereof - Google Patents
Inorganic organic intercalation superlattice film of large area flexible and preparation method thereof Download PDFInfo
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- 230000002687 intercalation Effects 0.000 title abstract description 11
- 238000009830 intercalation Methods 0.000 title abstract description 11
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims description 11
- 239000011368 organic material Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910021389 graphene Inorganic materials 0.000 claims description 6
- 229910052711 selenium Inorganic materials 0.000 claims description 6
- 229910052714 tellurium Inorganic materials 0.000 claims description 6
- 229910052723 transition metal Inorganic materials 0.000 claims description 6
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000010410 layer Substances 0.000 claims description 4
- 150000003624 transition metals Chemical class 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 239000004065 semiconductor Substances 0.000 claims description 3
- 229910052798 chalcogen Inorganic materials 0.000 claims description 2
- 150000001787 chalcogens Chemical class 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910052738 indium Inorganic materials 0.000 claims description 2
- 239000011229 interlayer Substances 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000000320 mechanical mixture Substances 0.000 claims 2
- 150000001408 amides Chemical class 0.000 claims 1
- 238000003475 lamination Methods 0.000 claims 1
- 238000003801 milling Methods 0.000 claims 1
- 230000007704 transition Effects 0.000 claims 1
- 238000001338 self-assembly Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000002841 Lewis acid Substances 0.000 abstract description 2
- 150000007517 lewis acids Chemical class 0.000 abstract description 2
- 230000005619 thermoelectricity Effects 0.000 abstract description 2
- 229910004211 TaS2 Inorganic materials 0.000 description 14
- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 description 8
- 229910010272 inorganic material Inorganic materials 0.000 description 4
- 239000011147 inorganic material Substances 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
- 229910052961 molybdenite Inorganic materials 0.000 description 3
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- -1 Transition Metal Sulfur Compounds Chemical class 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000002648 laminated material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 229910003092 TiS2 Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0234—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds
- B01J31/0235—Nitrogen containing compounds
- B01J31/0245—Nitrogen containing compounds being derivatives of carboxylic or carbonic acids
- B01J31/0247—Imides, amides or imidates (R-C=NR(OR))
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/34—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of chromium, molybdenum or tungsten
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/36—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of vanadium, niobium or tantalum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- 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
- C01B21/0605—Binary compounds of nitrogen with carbon
-
- 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
- C01B21/064—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 boron
-
- 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
-
- 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
- C01B32/198—Graphene oxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G35/00—Compounds of tantalum
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The present invention is raw material using polycrystalline stratiform inorganic powder, realize the organic intercalation that react based on lewis acid using the method for mechanical lapping, using in organic solution self assembly, be dried in vacuo and etc. obtain large area flexible inorganic lamellar material base organic molecule intercalation film.The film has the inorganic superlattice structure of inorganic-organic-.The preparation method is at low cost, high-efficient.In addition, the size of the film can be adjusted by adjusting the bottom size of self assembly container.Prepared hybrid film has many advantages, such as high conductivity, high electromagnetic shielding performance, high thermoelectricity capability, has practical value, is expected to realize commercial applications in Novel electronic devices.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to there is flexible inorganic stratified material base to have for a kind of large area
Machine transplanting of rice layer superlattice film and preparation method thereof.
Background technique
There is the report of many preparation inorganic material organic intercalation materials after the 1980s.But what wherein most used
Basis material is monocrystalline, and intercalation method is to be immersed in monocrystalline in organic solution to heat a couple of days or dozens of days.The growth of monocrystalline is special
Not time-consuming and higher cost, in addition the size of prepared intercalation material is limited by monocrystal material, therefore this with monocrystalline
It is low for the intercalation technique practical level of raw material.Later period, which has been reported that, has used polycrystalline layered inorganic material as original material, but
It is obtained product is powder.Traditional PM technique is difficult this kind of intercalation powder densification to block.Due to each
The random orientation and weak interaction of anisotropy powder, the block conductivity for suppressing the acquisition of such powder at room temperature are extremely low.This hair
Bright to use polycrystal powder for raw material, only realizing using only the method for mechanical lapping has the machine transplanting of rice based on lewis acid reaction
Layer, takes tens of minutes.In organic solution after self assembly, the inorganic lamellar material of large area flexible is can be obtained in vacuum drying
Base organic intercalation film.
Summary of the invention
To achieve the goals above, the present invention proposes following technical scheme.
A kind of Inorganic whisker film, comprising: inorganic lamellar material and organic material.It is organic in the laminated film
Material is located at the interlayer of inorganic lamellar material, forms the sandwich formats of " inorganic layer-organic layer-inorganic layer ".Inorganic laminated material
The content of material is 60.0~99.9wt%, and wherein wt% is with laminated film total weight, namely with organic matter and inorganic laminated material
Expect total weight.The inorganic lamellar material is graphene (graphene), graphene oxide (graphene oxide), six sides
BN (Hexagonal Boron Nitride), graphite phase carbon nitride (Graphitic Carbon Nitride), Transition Metal Sulfur
Compounds of group (Transition Metal Dichalcogenides, MX2Structure, wherein M Mo, W, Zr, Ta, V, Cr, Nb
Magnesium-yttrium-transition metal, the chalcogens such as X S, Se, Te), III-VI layered semiconductor (III-VI Layered
Semiconductors, MX structure, wherein M=Ga, In；X=S, Se, Te or M2X3Structure, wherein M=Bi；X=S, Se,
Te), transition metal carbide organic matter is organic amine molecules such as dimethyl sulfoxide, N-METHYLFORMAMIDE, n-hexylamine.It is described compound
Material film shape.
Another object of the present invention is to provide a kind of methods for preparing laminated film of the invention, i.e., first by layered inorganic
Material powder and organic material mechanical lapping mixing, after powdered inorganic material sufficiently expands, the ultrasonic disperse in organic solution
Form evenly dispersed liquid composition；Then liquid composition is obtained into composite film material after being centrifuged, being dried in vacuo.
In the preparation process in accordance with the present invention, the content of inorganic lamellar material be 40.0~99.9wt%, preferably 80.0~
The content of 99.8wt%, organic material are 0.1~40.0wt%, and preferably 0.2~20.0wt%, wherein wt% is with laminated film
Total weight.
In the preparation process in accordance with the present invention, it is preferred that first mix Solid inorganic stratified material powder and organic material
Mechanical lapping 0.1-2h afterwards forms adequately expanded combination powder；Said combination powder is transferred to ultrasound point in organic solution
0.5-10h is dissipated, fully dispersed liquid composition is formed；After above-mentioned composition 1000-10000 revolution per second is centrifuged 0.1-0.5h
Obtain composition clear liquid；Above-mentioned clear liquid is transferred in the smooth container in bottom, dry 1 in 60~200 DEG C of vacuum drying ovens~
72h to get arrive composite film material.
Beneficial effects of the present invention: preparation method of the invention is at low cost, high-efficient.The size of prepared hybrid film can
To be adjusted by the bottom size for adjusting self assembly container.Prepared hybrid film has high conductivity, high electromagnetic shielding
Many advantages, such as performance, high thermoelectricity capability, high electric catalyticing characteristic, has practical value, is expected to realize in Novel electronic devices
Commercial applications.
Detailed description of the invention
Fig. 1 is TaS2HA0.371NMF0.135The XRD diagram of film.
Fig. 2 is TaS2HA0.371NMF0.135The conductivity of film varies with temperature relational graph.
Fig. 3 is TaS2HA0.371NMF0.135The shield effectiveness figure of film.
Fig. 4 is TaS2HA0.371NMF0.135The flexible test figure of film.
Fig. 5 is TaS2HA0.371NMF0.135The stability test figure of film.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples.
After Solid inorganic stratified material powder and organic material mechanical lapping 0.1-2h, adequately expanded composition powder is formed
End；Said combination powder is transferred to ultrasonic disperse 0.5-10h in organic solution, forms fully dispersed liquid composition；It will
Composition clear liquid is obtained after above-mentioned composition 1000-10000 revolution per second centrifugation 0.1-0.5h；Above-mentioned clear liquid is transferred to bottom to put down
In whole container, which is transferred in vacuum oven, dries 1~72h in 60~200 DEG C of vacuum drying ovens to get arriving
Laminated film.
Fig. 1 is TaS2HA0.371NMF0.135The XRD diagram of film, XRD show that the interlamellar spacing after its intercalation is 1.033nm.
Fig. 2 is TaS2HA0.371NMF0.135The conductivity of film varies with temperature relational graph, and the conductivity of the film is to temperature
It increases and reduces, show metallic conduction attribute, conductivity is about 1200Scm at room temperature-1。
Fig. 3 is TaS2HA0.371NMF0.135The shield effectiveness figure of film, the electromagnet shield effect of the film are up to
31db。
Fig. 4 is TaS2HA0.371NMF0.135The flexible test figure of film, the film is when bending radius reaches 3mm, resistivity
Variation is less than 5%.
Fig. 5 is TaS2HA0.371NMF0.135The stability test figure of film, the film start to occur in 140 degrees centigrades
Weightlessness has good stability.
Embodiment 1:TaS2HA0.371NMF0.135And preparation method thereof
Weigh 0.4g TaS2It is added in mortar, weighs 1ml n-hexylamine solution and TaS2Powder mixing, hand-ground 30 are divided
Clock.Obtained powder is transferred in the vial equipped with 30ml N-METHYLFORMAMIDE after ultrasound 1 hour, 6000 revolutions per minute
It Zhongli's heart 10 minutes, takes in the be transferred to culture dish of supernatant liquor, is dried in vacuo at 130 DEG C 5 hours and obtains
TaS2HA0.371NMF0.135Film.
Embodiment 2:MoS2HA0.245NMF0.334And preparation method thereof
Weigh 0.5g MoS2It is added in mortar, weighs 1.5ml n-hexylamine solution and mixed with TiS2 powder, hand-ground
40 minutes.Obtained powder is transferred in the vial equipped with 40ml N-METHYLFORMAMIDE after ultrasound 30 minutes, 5000 turns
Centrifugation 20 minutes per minute, take in the be transferred to culture dish of supernatant liquor, are dried in vacuo at 120 DEG C 4 hours and obtain
MoS2HA0.245NMF0.334Film.
Embodiment 3:GOHA0.453NMF0.155And preparation method thereof
It weighs 1g GO to be added in mortar, weighs 2ml n-hexylamine solution and mixed with GO powder, hand-ground 50 minutes.It will
Obtained powder is transferred in the vial equipped with 40ml N-METHYLFORMAMIDE ultrasound after ten minutes, 3000 rpms from
It the heart 20 minutes, takes in the be transferred to culture dish of supernatant liquor, is dried in vacuo at 110 DEG C 6 hours and obtains GOHA0.453NMF0.155
Film.
Technical solution of the present invention is described in detail in above-described embodiment.It is apparent that the present invention is not limited being retouched
The embodiment stated.Based on the embodiments of the present invention, those skilled in the art can also make a variety of variations accordingly, but appoint
What is equal with the present invention or similar variation shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of Inorganic whisker film characterized by comprising inorganic lamellar material and organic material；In the THIN COMPOSITE
In film, organic material is located at the interlayer of inorganic lamellar material, forms the sandwich lamination knot of " inorganic layer-organic layer-inorganic layer "
Structure, wherein the content of inorganic lamellar material is 60.0~99.9wt% with laminated film total weight.
2. film as described in claim 1, which is characterized in that the inorganic lamellar material is graphene, graphene oxide, six
Square BN, graphite phase carbon nitride, Transition-metal dichalcogenide MX2Structure, wherein M Mo, W, Zr, Ta, V, Cr, Nb transition group
Metal, X S, Se, Te chalcogen, III-VI layered semiconductor MX structure, wherein M=Ga, In；X=S, Se, Te or M2X3
Structure, wherein M=Bi；X=S, Se, Te or transition metal carbide；The organic material is dimethyl sulfoxide, N- methyl first
Amide, n-hexylamine.
3. the manufacturing method of Inorganic whisker film as claimed in claim 1 or 2, which is characterized in that the manufacturing method includes
Following steps:
1) it by inorganic lamellar material powder and organic material mechanical mixture and grinds；
2) after inorganic lamellar material powder sufficiently expands, ultrasonic disperse forms evenly dispersed liquid combination in organic solution
Object；
3) liquid composition is then obtained into composite film material after being centrifuged, being dried in vacuo.
4. method as claimed in claim 3, which is characterized in that the content of the inorganic lamellar material is with laminated film total weight
Meter is 80.0~99.8wt%.
5. method as claimed in claim 3, which is characterized in that the content of the organic material with laminated film total weight,
For 0.1~40.0wt%.
6. method as claimed in claim 3, which is characterized in that the content of the organic material is with laminated film total weight
0.2~20.0wt%.
7. method as claimed in claim 3, which is characterized in that simultaneously milling time is 0.1-2h to the mechanical mixture.
8. method as claimed in claim 3, which is characterized in that the ultrasonic disperse time is 0.5-10h.
9. method as claimed in claim 3, which is characterized in that the speed of the centrifugation and time are respectively that 1000-10000 turns
Per second and 0.1-2h.
10. method as claimed in claim 3, which is characterized in that the vacuum drying temperature and time is respectively 60-200
DEG C and 1-72h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111468104A (en) * | 2019-10-15 | 2020-07-31 | 中山大学 | Preparation method and application of graphene-bismuth tungstate |
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| CN111468104B (en) * | 2019-10-15 | 2021-07-16 | 中山大学 | Preparation method and application of graphene-bismuth tungstate |
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