CN103496692B - A kind of method utilizing liquefied ammonia/alkali metal soln to prepare two-dimension nano materials - Google Patents
A kind of method utilizing liquefied ammonia/alkali metal soln to prepare two-dimension nano materials Download PDFInfo
- Publication number
- CN103496692B CN103496692B CN201310424537.6A CN201310424537A CN103496692B CN 103496692 B CN103496692 B CN 103496692B CN 201310424537 A CN201310424537 A CN 201310424537A CN 103496692 B CN103496692 B CN 103496692B
- Authority
- CN
- China
- Prior art keywords
- nano materials
- ammonia
- dimension nano
- liquefied ammonia
- prepare
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Utilize liquefied ammonia/alkali metal soln to prepare a method for two-dimension nano materials, it relates to the preparation method of two-dimension nano materials.The present invention will solve the problem that product yield is low and intercalation process is restive that existing two-dimension nano materials preparation method obtains, preparation method: the basic metal one, taken and lamellar compound put into silica tube; Two, silica tube is filled with high-purity ammonia after vacuumizing, and is cooled to the ammonia liquefaction in pipe; Three, oscillator quartz pipe takes off to the blueness of liquid ammonia solution, then extracts the liquefied ammonia of vaporization out; Four, the lamellar compound after intercalation is put into deionized water for ultrasonic process; Five, the nano material aqueous solution of step 4 is put into whizzer centrifugal, collect in supernatant liquid and obtain two-dimension nano materials.The productive rate being obtained two-dimension nano materials by preparation method of the present invention can reach 80%, and gradually becomes colourless process by observing liquid ammonia solution color by blueness, effectively controls alkalimetal ion to the intercalation process of lamellar compound.
Description
Technical field
The present invention relates to a kind of preparation method of two-dimension nano materials.
Background technology
Two-dimension nano materials receives the common concern of people because its important Theory and applications is worth.For Graphene, it is made up of monolayer carbon atom, and this material shows high electron mobility (200000cm
2v
-1s
-1), ultrafast Fermi velocity (~ 1.0 × 10
8m/s), high thermal conductivity (5000W/mK) and high Young's modulus (1.0 × 10
14the excellent properties such as Pa), has a wide range of applications at numerous areas such as nanoelectronic, photo-detector, ultracapacitor and catalysis.Another kind of typical two-dimension nano materials is single or multiple lift molybdenumdisulphide, and the structure and electronic properties of its excellence makes it in energy storage, catalysis etc., have important application prospect.Therefore, people wish to develop more two-dimension nano materials, to investigate their abundant physicochemical property.
Two-dimension nano materials is normally prepared by peeling layered compounds, so-called lamellar compound, refer to that the atom in layer combines with stronger covalent linkage or ionic linkage effect, and interlayer is a large compounds of relatively weak Van der Waals force, therefore corresponding nanometer sheet can be obtained by destroying its interlayer Van der Waals force.The method preparing two-dimension nano materials at present mainly comprises mechanically peel, ultrasonic and ion insertion stripping of liquid phase etc., but, these preparation methods also exist problems, such as: (1) productive rate is lower, the productive rate of mechanically peel method is lower than 10%, and the productive rate of liquid phase ultrasonic method is usually less than 50%; (2) time is longer, generally needs consuming time tens of little of a couple of days; (3) environmental problem, liquid phase ultrasonic method needs to use the organic solvent easily polluted environment; (4) restive, stripping or intercalation process cannot control effectively.
Publication number is CN102320598, denomination of invention is reacted adopting the graphite oxide of the Hummer method of Hummer method or improvement acquisition to add to be dissolved with in alkali-metal liquid nitrogen solution for describing in " a kind of preparation method of Graphene ", subsequent purification is separated, thus prepares Graphene.
Summary of the invention
The object of the invention is to solve the problem that product yield is low and intercalation process is restive that existing two-dimension nano materials preparation method obtains, and a kind of method utilizing liquefied ammonia/alkali metal soln to prepare two-dimension nano materials is provided.
The method that the present invention utilizes liquefied ammonia/alkali metal soln to prepare two-dimension nano materials follows these steps to realize:
One, be that 1 ︰ (1 ~ 10) takes basic metal and lamellar compound in molar ratio under the environment of protection of inert gas, then put into silica tube;
Two, silica tube is evacuated to 10
-4be filled with the ammonia that purity is 99.9999% after Pa, then cool silica tube to the ammonia liquefaction in pipe, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, oscillator quartz pipe, carries out continuing cooling to silica tube in the process of oscillator quartz pipe, and the blueness of vibrating to liquid ammonia solution is taken off, and the liquefied ammonia extracting out of then at room temperature vaporizing, obtains the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained puts into deionized water for ultrasonic 1 ~ 2h, obtains the nano material aqueous solution;
Five, the nano material aqueous solution of step 4 is put into whizzer centrifugal, then collect in supernatant liquid after centrifugation and obtain two-dimension nano materials;
Basic metal wherein described in step one is lithium, sodium or potassium;
Described lamellar compound is graphite, Vanadium Pentoxide in FLAKES, molybdic oxide, hexagonal boron nitride, metal disulfides MX
2(wherein M=Sn, Ti, Zr, Hf, V, Nb, Ta, Mo or W, X=S, Se or Te), Hofmann type compound N i (CN)
2nH
3, kaolinite, dickite, agalmatolite, hydrotalcite (LDHs), houghite, transition metal oxide YO
2(wherein Y=Ti, V, Cr, Mn, Fe, Co or Ni), graphite phase carbon nitride, montmorillonite, saponite, vermiculite or rhombspar.
The present invention adopts the basic metal being dissolved in liquefied ammonia to carry out intercalation to lamellar compound, and the compound after intercalation is ultrasonic in deionized water, realizes the effective stripping to lamellar compound, thus prepares ultra-thin two-dimension nano material.
Compared with existing stripping means, the method that the present invention prepares two-dimension nano materials has method simply, and the advantage that speed of response is fast and productive rate is higher, the number of plies of the two-dimension nano materials obtained is 1 ~ 10 layer, and productive rate can reach 80%.The intercalation speed of alkalimetal ion can be regulated by the frequency changing oscillator quartz pipe simultaneously, especially, maximum feature of the present invention is faded for colourless process by observing liquid ammonia solution color gradually by mazarine, effectively controls alkalimetal ion to the intercalation process of lamellar compound.
Accompanying drawing explanation
Fig. 1 is the atomic force microscope figure of the molybdenum disulfide nano sheet that embodiment two obtains;
Fig. 2 is the atomic force microscope figure of the tungsten disulfide nano slices that embodiment three obtains;
Fig. 3 is the transmission electron microscope figure (TransmissionElectronMicroscopy, TEM) of the graphite phase carbon nitride nanometer sheet that embodiment eight obtains;
Fig. 4 is the high resolution transmission electron microscopy figure (HighResolutionTransmissionElectronMicroscopy, HRTEM) of the graphite phase carbon nitride nanometer sheet that embodiment eight obtains;
Fig. 5 is the atomic force microscope figure (AtomicForceMicroscopy, AFM) of the graphite phase carbon nitride nanometer sheet that embodiment eight obtains.
Embodiment
Embodiment one: the method that present embodiment utilizes liquefied ammonia/alkali metal soln to prepare two-dimension nano materials follows these steps to realize:
One, be that 1 ︰ (1 ~ 10) takes basic metal and lamellar compound in molar ratio under the environment of protection of inert gas, then put into silica tube;
Two, silica tube is evacuated to 10
-4be filled with the ammonia that purity is 99.9999% after Pa, then cool silica tube to the ammonia liquefaction in pipe, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, oscillator quartz pipe, carries out continuing cooling to silica tube in the process of oscillator quartz pipe, and the blueness of vibrating to liquid ammonia solution is taken off, and the liquefied ammonia extracting out of then at room temperature vaporizing, obtains the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained puts into deionized water for ultrasonic 1 ~ 2h, obtains the nano material aqueous solution;
Five, the nano material aqueous solution of step 4 is put into whizzer centrifugal, then collect in supernatant liquid after centrifugation and obtain two-dimension nano materials;
Basic metal wherein described in step one is lithium, sodium or potassium;
Described lamellar compound is graphite, Vanadium Pentoxide in FLAKES, molybdic oxide, hexagonal boron nitride, metal disulfides MX
2, (wherein M=Sn, Ti, Zr, Hf, V, Nb, Ta, Mo or W, X=S, Se or Te), Hofmann type compound N i (CN)
2nH
3, kaolinite, dickite, agalmatolite, hydrotalcite (LDHs), houghite, transition metal oxide YO
2(wherein Y=Ti, V, Cr, Mn, Fe, Co or Ni), graphite phase carbon nitride, montmorillonite, saponite, vermiculite or rhombspar.
Present embodiment makes the alkalimetal ion in liquefied ammonia insert lamellar compound gradually by step 3 by oscillator quartz pipe, and the time of general oscillator quartz pipe is 20min to 1h.Step 4 puts at lamellar compound the generation that deionized water ultrasonic procedure can be observed bubble.It is to remove large-size particle that step 5 is put into whizzer centrifugal.
The general formula of the hydrotalcite in present embodiment lamellar compound is [Mg
1-xm
x iII(OH)
2] [A
x/n] mH
2o, wherein M
iIIfor ionic radius and the close trivalent metal ion of magnesium ion, as M
iII=Al
3+, Cr
3+, Co
3+, Fe
3+, Sc
3+or V
3+, A
n-for negatively charged ion, as A
n-=CO
3 2-, NO
3 -, F
-, Cl
-, Br
-, I
-, CrO
4 2-, H
2pO
4 -, PO
4 3-, SO
4 2-or SO
3 2-; The general formula of houghite is [M
1-x iIm
x iII(OH)
2] [A
x/n] mH
2o, wherein M
iI=Mg, Fe, Co, Ni, Mn or Zn, M
iII=Al, Fe, Cr, Mn or V; A
n-for negatively charged ion, as A
n-=CO
3 2-, NO
3 -, F
-, Cl
-, Br
-, I
-, CrO
4 2-, H
2pO
4 -, PO
4 3-, SO
4 2-or SO
3 2-.
Embodiment two: present embodiment and embodiment one are not less than 99.9% unlike the alkali-metal purity described in step one.Other step and parameter identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two are not less than 99.9% unlike the purity of the lamellar compound described in step one.Other step and parameter identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three are that 1 ︰ 2 takes basic metal and lamellar compound in molar ratio unlike step one under the environment of protection of inert gas.Other step and parameter identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four are adopt cooled with liquid nitrogen or adopt the mixture of ice and water of ethanol and water to cool unlike the type of cooling of the cooling silica tube described in step 2.Other step and parameter identical with one of embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five are unlike putting into centrifuge described in step 5, and wherein centrifugal speed is 3000r/min ~ 15000r/min.Other step and parameter identical with one of embodiment one to five.
Embodiment one: the method that the present embodiment utilizes liquefied ammonia/alkali metal soln to prepare two-dimension nano materials follows these steps to realize:
One, in the glove box of argon shield, take the powdered graphite of 0.005mol metallic lithium and 0.01mol, then put into silica tube;
Two, silica tube is evacuated to 10
-4be filled with the ammonia that purity is 99.9999% after Pa, then liquefy to the ammonia in pipe with cooled with liquid nitrogen silica tube, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, oscillator quartz pipe, carries out continuing cooling to silica tube in the process of oscillator quartz pipe, and the blueness of vibrating to liquid ammonia solution is taken off, and the liquefied ammonia extracting out of then at room temperature vaporizing, obtains the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained puts into deionized water for ultrasonic 1.5h, obtains the nano material aqueous solution;
Five, the nano material aqueous solution of step 4 is put into whizzer with the centrifugation of 4000r/min, then collect in supernatant liquid after centrifugation and obtain two-dimension nano materials.
After the present embodiment step 3 vibration 30min, the blueness of liquid ammonia solution is taken off.
The two-dimension nano materials that the present embodiment obtains is two-dimensional nano-graphene.
Embodiment two: the method that the present embodiment utilizes liquefied ammonia/alkali metal soln to prepare two-dimension nano materials follows these steps to realize:
One, in the glove box of argon shield, take the molybdenum disulfide powder of 0.005mol metallic lithium and 0.01mol, then put into silica tube;
Two, silica tube is evacuated to 10
-4be filled with the ammonia that purity is 99.9999% after Pa, then liquefy to the ammonia in pipe with cooled with liquid nitrogen silica tube, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, oscillator quartz pipe, carries out continuing cooling to silica tube in the process of oscillator quartz pipe, and the blueness of vibrating to liquid ammonia solution is taken off, and the liquefied ammonia extracting out of then at room temperature vaporizing, obtains the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained puts into deionized water for ultrasonic 1.5h, obtains the nano material aqueous solution;
Five, the nano material aqueous solution of step 4 is put into whizzer with the centrifugation of 4000r/min, then collect in supernatant liquid after centrifugation and obtain two-dimension nano materials.
After the present embodiment step 3 vibration 30min, the blueness of liquid ammonia solution is taken off.
The two-dimension nano materials that the present embodiment obtains is molybdenum disulfide nano sheet, and as shown in Figure 1, in figure, the thickness of dotted line place nanometer sheet is about 3.5nm to the image under its atomic force microscope.
Embodiment three: the method that the present embodiment utilizes liquefied ammonia/alkali metal soln to prepare two-dimension nano materials follows these steps to realize:
One, in the glove box of argon shield, take the tungsten disulphide powder of 0.005mol metallic lithium and 0.01mol, then put into silica tube;
Two, silica tube is evacuated to 10
-4be filled with the ammonia that purity is 99.9999% after Pa, then liquefy to the ammonia in pipe with cooled with liquid nitrogen silica tube, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, oscillator quartz pipe, carries out continuing cooling to silica tube in the process of oscillator quartz pipe, and the blueness of vibrating to liquid ammonia solution is taken off, and the liquefied ammonia extracting out of then at room temperature vaporizing, obtains the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained puts into deionized water for ultrasonic 1.5h, obtains the nano material aqueous solution;
Five, the nano material aqueous solution of step 4 is put into whizzer with the centrifugation of 4000r/min, then collect in supernatant liquid after centrifugation and obtain two-dimension nano materials.
After the present embodiment step 3 vibration 30min, the blueness of liquid ammonia solution is taken off.
The two-dimension nano materials that the present embodiment obtains is tungsten disulfide nano slices, and as shown in Figure 2, in figure, the thickness of dotted line place nanometer sheet is about 3.0nm to the image under its atomic force microscope.
Embodiment four: the method that the present embodiment utilizes liquefied ammonia/alkali metal soln to prepare two-dimension nano materials follows these steps to realize:
One, in the glove box of argon shield, take the titanium disulfide powder of 0.005mol metallic lithium and 0.01mol, then put into silica tube;
Two, silica tube is evacuated to 10
-4be filled with the ammonia that purity is 99.9999% after Pa, then liquefy to the ammonia in pipe with cooled with liquid nitrogen silica tube, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, oscillator quartz pipe, carries out continuing cooling to silica tube in the process of oscillator quartz pipe, and the blueness of vibrating to liquid ammonia solution is taken off, and the liquefied ammonia extracting out of then at room temperature vaporizing, obtains the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained puts into deionized water for ultrasonic 1.5h, obtains the nano material aqueous solution;
Five, the nano material aqueous solution of step 4 is put into whizzer with the centrifugation of 4000r/min, then collect in supernatant liquid after centrifugation and obtain two-dimension nano materials.
After the present embodiment step 3 vibration 30min, the blueness of liquid ammonia solution is taken off.
The two-dimension nano materials that the present embodiment obtains is titanium disulfide nanometer sheet, and the productive rate of the present embodiment is 80%.
Embodiment five: the method that the present embodiment utilizes liquefied ammonia/alkali metal soln to prepare two-dimension nano materials follows these steps to realize:
One, in the glove box of argon shield, take the two telluride molybdenum powder of 0.005mol metallic lithium and 0.01mol, then put into silica tube;
Two, silica tube is evacuated to 10
-4be filled with the ammonia that purity is 99.9999% after Pa, then liquefy to the ammonia in pipe with cooled with liquid nitrogen silica tube, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, oscillator quartz pipe, carries out continuing cooling to silica tube in the process of oscillator quartz pipe, and the blueness of vibrating to liquid ammonia solution is taken off, and the liquefied ammonia extracting out of then at room temperature vaporizing, obtains the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained puts into deionized water for ultrasonic 1.5h, obtains the nano material aqueous solution;
Five, the nano material aqueous solution of step 4 is put into whizzer with the centrifugation of 4000r/min, then collect in supernatant liquid after centrifugation and obtain two-dimension nano materials.
After the present embodiment step 3 vibration 30min, the blueness of liquid ammonia solution is taken off.
The two-dimension nano materials that the present embodiment obtains is two telluride molybdenum nanometer sheet.
Embodiment six: the method that the present embodiment utilizes liquefied ammonia/alkali metal soln to prepare two-dimension nano materials follows these steps to realize:
One, in the glove box of argon shield, take the two selenizing molybdenum powder of 0.005mol metallic lithium and 0.01mol, then put into silica tube;
Two, silica tube is evacuated to 10
-4be filled with the ammonia that purity is 99.9999% after Pa, then liquefy to the ammonia in pipe with cooled with liquid nitrogen silica tube, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, oscillator quartz pipe, carries out continuing cooling to silica tube in the process of oscillator quartz pipe, and the blueness of vibrating to liquid ammonia solution is taken off, and the liquefied ammonia extracting out of then at room temperature vaporizing, obtains the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained puts into deionized water for ultrasonic 1.5h, obtains the nano material aqueous solution;
Five, the nano material aqueous solution of step 4 is put into whizzer with the centrifugation of 4000r/min, then collect in supernatant liquid after centrifugation and obtain two-dimension nano materials.
After the present embodiment step 3 vibration 30min, the blueness of liquid ammonia solution is taken off.
The two-dimension nano materials that the present embodiment obtains is two selenizing molybdenum nanometer sheet, and the productive rate of the present embodiment is 80%.
Embodiment seven: the method that the present embodiment utilizes liquefied ammonia/alkali metal soln to prepare two-dimension nano materials follows these steps to realize:
One, in the glove box of argon shield, take the two tungsten selenide powder of 0.005mol metallic lithium and 0.01mol, then put into silica tube;
Two, silica tube is evacuated to 10
-4be filled with the ammonia that purity is 99.9999% after Pa, then liquefy to the ammonia in pipe with cooled with liquid nitrogen silica tube, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, oscillator quartz pipe, carries out continuing cooling to silica tube in the process of oscillator quartz pipe, and the blueness of vibrating to liquid ammonia solution is taken off, and the liquefied ammonia extracting out of then at room temperature vaporizing, obtains the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained puts into deionized water for ultrasonic 1.5h, obtains the nano material aqueous solution;
Five, the nano material aqueous solution of step 4 is put into whizzer with the centrifugation of 4000r/min, then collect in supernatant liquid after centrifugation and obtain two-dimension nano materials.
After the present embodiment step 3 vibration 30min, the blueness of liquid ammonia solution is taken off.
The two-dimension nano materials that the present embodiment obtains is two tungsten selenide nanometer sheet.
Embodiment eight: the method that the present embodiment utilizes liquefied ammonia/alkali metal soln to prepare two-dimension nano materials follows these steps to realize:
One, in the glove box of argon shield, take the graphite phase carbon nitride powder of 0.005mol metallic lithium and 0.01mol, then put into silica tube;
Two, silica tube is evacuated to 10
-4be filled with the ammonia that purity is 99.9999% after Pa, then liquefy to the ammonia in pipe with cooled with liquid nitrogen silica tube, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, oscillator quartz pipe, carries out continuing cooling to silica tube in the process of oscillator quartz pipe, and the blueness of vibrating to liquid ammonia solution is taken off, and the liquefied ammonia extracting out of then at room temperature vaporizing, obtains the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained puts into deionized water for ultrasonic 1.5h, obtains the nano material aqueous solution;
Five, the nano material aqueous solution of step 4 is put into whizzer with the centrifugation of 4000r/min, then collect in supernatant liquid after centrifugation and obtain two-dimension nano materials.
After the present embodiment step 3 vibration 30min, the blueness of liquid ammonia solution is taken off.
The two-dimension nano materials that the present embodiment obtains is graphite phase carbon nitride nanometer sheet, its transmission electron microscope figure as shown in Figure 3 and Figure 4, as shown in Figure 5, wherein in Fig. 5, the thickness of dotted line place nanometer sheet is about 2.5nm to atomic force microscope figure, and the spacing of each layer is 0.35nm.The productive rate of the present embodiment is 80%.
Shown by above embodiment, utilize the basic metal being dissolved in liquefied ammonia to carry out intercalation to lamellar compound, and the compound after intercalation is ultrasonic in deionized water, effectively can realize the stripping to lamellar compound, prepare ultra-thin two-dimension nano materials.
Claims (6)
1. utilize liquefied ammonia/alkali metal soln to prepare a method for two-dimension nano materials, it is characterized in that the method utilizing liquefied ammonia/alkali metal soln to prepare two-dimension nano materials follows these steps to realize:
One, be that 1 ︰ (1 ~ 10) takes basic metal and lamellar compound in molar ratio under the environment of protection of inert gas, then put into silica tube;
Two, silica tube is evacuated to 10
-4be filled with the ammonia that purity is 99.9999% after Pa, then cool silica tube to the ammonia liquefaction in pipe, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, oscillator quartz pipe, carries out continuing cooling to silica tube in the process of oscillator quartz pipe, and the blueness of vibrating to liquid ammonia solution is taken off, and the liquefied ammonia extracting out of then at room temperature vaporizing, obtains the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained puts into deionized water for ultrasonic 1 ~ 2h, generates bubble, obtains the nano material aqueous solution;
Five, the nano material aqueous solution of step 4 is put into whizzer centrifugal, then collect in supernatant liquid after centrifugation and obtain two-dimension nano materials;
Basic metal wherein described in step one is lithium, sodium or potassium;
Described lamellar compound is graphite, Vanadium Pentoxide in FLAKES, molybdic oxide, hexagonal boron nitride, metal disulfides MX
2, Hofmann type compound N i (CN)
2nH
3, kaolinite, dickite, agalmatolite, hydrotalcite, houghite, transition metal oxide YO
2, graphite phase carbon nitride, montmorillonite, saponite, vermiculite or rhombspar; Wherein metal disulfides MX
2in M=Sn, Ti, Zr, Hf, V, Nb, Ta, Mo or W, X=S, Se or Te, transition metal oxide YO
2in Y=Ti, V, Cr, Mn, Fe, Co or Ni.
2. a kind of method utilizing liquefied ammonia/alkali metal soln to prepare two-dimension nano materials according to claim 1, is characterized in that the alkali-metal purity described in step one is not less than 99.9%.
3. a kind of method utilizing liquefied ammonia/alkali metal soln to prepare two-dimension nano materials according to claim 1, is characterized in that the purity of the lamellar compound described in step one is not less than 99.9%.
4. a kind of method utilizing liquefied ammonia/alkali metal soln to prepare two-dimension nano materials according to claim 1, is characterized in that step one is that 1 ︰ 2 takes basic metal and lamellar compound in molar ratio under the environment of protection of inert gas.
5. a kind of method utilizing liquefied ammonia/alkali metal soln to prepare two-dimension nano materials according to claim 1, is characterized in that the type of cooling of the cooling silica tube described in step 2 adopts cooled with liquid nitrogen or adopts the mixture of ice and water of ethanol and water to cool.
6. a kind of method utilizing liquefied ammonia/alkali metal soln to prepare two-dimension nano materials according to claim 1, it is characterized in that putting into centrifuge described in step 5, wherein centrifugal speed is 3000r/min ~ 15000r/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310424537.6A CN103496692B (en) | 2013-09-17 | 2013-09-17 | A kind of method utilizing liquefied ammonia/alkali metal soln to prepare two-dimension nano materials |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310424537.6A CN103496692B (en) | 2013-09-17 | 2013-09-17 | A kind of method utilizing liquefied ammonia/alkali metal soln to prepare two-dimension nano materials |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103496692A CN103496692A (en) | 2014-01-08 |
| CN103496692B true CN103496692B (en) | 2016-02-10 |
Family
ID=49861986
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310424537.6A Active CN103496692B (en) | 2013-09-17 | 2013-09-17 | A kind of method utilizing liquefied ammonia/alkali metal soln to prepare two-dimension nano materials |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103496692B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6637895B2 (en) | 2014-02-17 | 2020-01-29 | ユーシーエル ビジネス リミテッド | Method for producing a dispersion of nanosheets |
| CN104402053B (en) * | 2014-11-04 | 2016-05-18 | 中国科学院大学 | The preparation method of one kind Graphene two-dimensional nano sheet |
| CN104743562A (en) * | 2015-03-20 | 2015-07-01 | 济宁利特纳米技术有限责任公司 | Preparation method of sericite nanosheets |
| CN108314021A (en) * | 2017-01-16 | 2018-07-24 | 山东恒华新材料有限公司 | The batch production method of high-quality graphene |
| CN110346430B (en) * | 2019-06-17 | 2021-06-04 | 福建师范大学 | Na+Doping with g-C3N4Composite material, electrochemical sensor, preparation method and application thereof |
| CN114348975A (en) * | 2021-03-10 | 2022-04-15 | 湖北大学 | Thermoelectric material for regulating p and n type conversion by SPS temperature and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320598A (en) * | 2011-07-26 | 2012-01-18 | 河南大学 | Preparation method of graphene |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008097343A2 (en) * | 2006-08-08 | 2008-08-14 | William Marsh Rice University | Functionalized graphene materials and method of production thereof |
-
2013
- 2013-09-17 CN CN201310424537.6A patent/CN103496692B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320598A (en) * | 2011-07-26 | 2012-01-18 | 河南大学 | Preparation method of graphene |
Non-Patent Citations (1)
| Title |
|---|
| Direct Synthesis of Lithium-Intercalated Graphene for Electrochemical Energy Storage Application;Ashavani Kumar et al.;《ACS NANO》;20110524;第5卷(第6期);4348页METHODS部分 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103496692A (en) | 2014-01-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103496692B (en) | A kind of method utilizing liquefied ammonia/alkali metal soln to prepare two-dimension nano materials | |
| Li et al. | A self-healing layered GeP anode for high-performance Li-ion batteries enabled by low formation energy | |
| Wang et al. | Facile, mild and fast thermal-decomposition reduction of graphene oxide in air and its application in high-performance lithium batteries | |
| Tang et al. | Hydrothermal synthesis and characterization of novel flowerlike MoS2 hollow microspheres | |
| Wang et al. | Rapid microwave-assisted hydrothermal synthesis of one-dimensional MoO3 nanobelts | |
| Yang et al. | Hydrothermal synthesis of MoO3 nanobelt‐graphene composites | |
| Fan et al. | Feasibility of using chemically exfoliated SnSe nanobelts in constructing flexible SWCNTs-based composite films for high-performance thermoelectric applications | |
| Yang et al. | A facile one-step hydrothermal method to produce graphene–MoO3 nanorod bundle composites | |
| CN101704552A (en) | Molybdenum disulfide nano tube and preparation method thereof | |
| Chen et al. | Large-scale synthesis of single-crystal molybdenum trioxide nanobelts by hot-wire chemical vapour deposition | |
| JP2019524612A (en) | Boron nitride nanomaterial, its production method and application | |
| Zhang et al. | Interface-induced enhanced electromagnetic wave absorption property of metal-organic frameworks wrapped by graphene sheets | |
| Thangasamy et al. | One-dimensional growth of hexagonal rods of metastable h-MoO3 using one-pot, rapid and environmentally benign supercritical fluid processing | |
| CN103771521B (en) | Method for preparing tungsten disulfide nano sheet | |
| Zhen et al. | A facile hydrothermal route to the large-scale synthesis of CoWO4 nanorods | |
| Li et al. | Enhanced Lithium Storage Performance of Liquid‐Phase Exfoliated Graphene Supported WS2 Heterojunctions | |
| Ni et al. | Ionic liquid-assisted solvothermal synthesis of hollow CoFe2O4 microspheres and their absorbing performances | |
| Zhang et al. | Core–shell SnO2@ TiO2–B nanowires as the anode of lithium ion battery with high capacity and rate capability | |
| KR20100013688A (en) | Aa' stacked graphite and the fabrication method thereof | |
| Chen et al. | Sodium-ion storage mechanisms and design strategies of molybdenum-based materials: A review | |
| He et al. | Growth of vertical MoS2 nanosheets on carbon materials by chemical vapor deposition: Influence of substrates | |
| Jia et al. | Facile synthesis of branched MoS2 nanowires | |
| Liang et al. | Hydrothermal synthesis and electrochemical performance of novel channel-structured β-Ag0. 33V2O5 nanorods | |
| Biswas et al. | Pressure-induced phase transitions in nanocrystalline ReO3 | |
| Geng et al. | Synthesis of hollow carbon nanospheres through a ZnSe nanoparticle template route |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |