CN103496692A - Method for preparing two-dimensional nanomaterial by utilizing liquid ammonia/alkali metal solution - Google Patents
Method for preparing two-dimensional nanomaterial by utilizing liquid ammonia/alkali metal solution Download PDFInfo
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- CN103496692A CN103496692A CN201310424537.6A CN201310424537A CN103496692A CN 103496692 A CN103496692 A CN 103496692A CN 201310424537 A CN201310424537 A CN 201310424537A CN 103496692 A CN103496692 A CN 103496692A
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Abstract
The invention provides a method for preparing a two-dimensional nanomaterial by utilizing a liquid ammonia/alkali metal solution and relates to a preparation method of a two-dimensional nanomaterial. The invention aims to solve the problems that a product obtained by the existing preparation method of the two-dimensional nanomaterial has low yield and the intercalation process is difficult to control. The preparation method comprises the following steps: 1, placing weighed alkali metal and lamellar compounds into a quartz tube; 2, vacuumizing the quartz tube, introducing high-purity amminia gas and cooling until the ammonia gas in the tube is liquefied; 3, oscillating the quartz tube until the blue color of the liquid ammonia solution is faded and extracting vaporized liquid ammonia; 4, placing the lamellar compounds after intercalation into deionized water and performing ultrasonic treatment; and 5, placing the nanomaterial aqueous solution in the step 4 into a centrifugal machine, centrifuging and collecting a supernate liquid to obtain the two-dimensional nanomaterial. The yield of the two-dimensional nanomaterial obtained by the preparation method provided by the invention can reach 80 percent, and the intercalation process of alkali metal ions on the lamellar compounds is effectively controlled by observing the process that the color of the liquid ammonia solution is gradually changed from blue to colorless.
Description
Technical field
The present invention relates to a kind of preparation method of two-dimensional nano material.
Background technology
The two-dimensional nano material is because its important theory and using value have been subject to people's common concern.Take Graphene as example, and it is comprised of the monolayer carbon atom, and this material has demonstrated 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
14pa) etc. excellent properties, have a wide range of applications at numerous areas such as nanoelectronic, photo-detector, ultracapacitor and catalysis.Another kind of typical two-dimensional nano material is single or multiple lift molybdenumdisulphide, and the structure and electronic properties of its excellence makes it at aspects such as energy storage, catalysis, have important application prospect.Therefore, people wish to develop more two-dimensional nano material, to investigate their abundant physicochemical property.
The two-dimensional nano material normally is 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 the large compounds that interlayer is relatively weak Van der Waals force, so can obtain corresponding nanometer sheet by destroying its interlayer Van der Waals force.The method for preparing at present the two-dimensional nano material mainly comprises mechanically peel, and the ultrasonic and ion intercalation of liquid phase is peeled off etc., yet, these preparation methods exist problems, for example: (1) productive rate is lower, and 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 longer, generally need tens of hours consuming time to a couple of days; (3) environmental problem, the liquid phase ultrasonic method need to be used the organic solvent that environment is easily polluted; (4) restive, peel off or the intercalation process can't control effectively.
Summary of the invention
The objective of the invention is to solve the low and restive problem of intercalation process of product yield that existing two-dimensional nano material preparation method obtains, and a kind of method of utilizing liquefied ammonia/alkali metal soln to prepare the two-dimensional nano material is provided.
The method that the present invention utilizes liquefied ammonia/alkali metal soln to prepare the two-dimensional nano material 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 cooling silica tube liquefies to the ammonia in pipe, and basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, the vibration silica tube continues coolingly in the process of vibration silica tube to silica tube, vibrates and takes off to the blueness of liquid ammonia solution, and then at room temperature vaporize liquefied ammonia extraction obtain the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained is put 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 to whizzer centrifugal, then in the supernatant liquid after centrifugal, collect and obtain the two-dimensional nano material;
Wherein the described basic metal of step 1 is lithium, sodium or potassium;
Described lamellar compound is graphite, Vanadium Pentoxide in FLAKES, molybdic oxide, hexagonal boron nitride, metal dithionite compound 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 carbonitride, montmorillonite, saponite, vermiculite or rhombspar.
The present invention adopts the basic metal be dissolved in liquefied ammonia to carry out intercalation to lamellar compound, and by the compound after intercalation in deionized water for ultrasonic, realize effectively the peeling off of lamellar compound, thereby prepare the ultra-thin two-dimension nano material.
With existing stripping means, compare, it is simple that the method that the present invention prepares the two-dimensional nano material has method, the fast and higher advantage of productive rate of speed of response, and the number of plies of the two-dimensional nano material obtained is 1～10 layer, productive rate can reach 80%.Simultaneously the intercalation speed of alkalimetal ion can be regulated by the vibrate frequency of silica tube of change, especially, maximum characteristics of the present invention are to be faded gradually for colourless process by mazarine by observing the liquid ammonia solution color, effectively control the intercalation process of alkalimetal ion to lamellar compound.
The accompanying drawing explanation
Fig. 1 is the atomic force microscope figure of the molybdenum disulfide nano sheet that obtains of embodiment bis-;
Fig. 2 is the atomic force microscope figure of the tungsten disulfide nano slices that obtains of embodiment tri-;
Fig. 3 is the transmission electron microscope figure (Transmission Electron Microscopy, TEM) of the graphite-phase azotized carbon nano sheet that obtains of embodiment eight;
Fig. 4 is the high resolution transmission electron microscopy figure (High Resolution Transmission Electron Microscopy, HRTEM) of the graphite-phase azotized carbon nano sheet that obtains of embodiment eight;
Fig. 5 is the atomic force microscope figure (Atomic Force Microscopy, AFM) of the graphite-phase azotized carbon nano sheet that obtains of embodiment eight.
Embodiment
Embodiment one: the method that present embodiment utilizes liquefied ammonia/alkali metal soln to prepare the two-dimensional nano material 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 cooling silica tube liquefies to the ammonia in pipe, and basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, the vibration silica tube continues coolingly in the process of vibration silica tube to silica tube, vibrates and takes off to the blueness of liquid ammonia solution, and then at room temperature vaporize liquefied ammonia extraction obtain the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained is put 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 to whizzer centrifugal, then in the supernatant liquid after centrifugal, collect and obtain the two-dimensional nano material;
Wherein the described basic metal of step 1 is lithium, sodium or potassium;
Described lamellar compound is graphite, Vanadium Pentoxide in FLAKES, molybdic oxide, hexagonal boron nitride, metal dithionite compound 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 carbonitride, montmorillonite, saponite, vermiculite or rhombspar.
Present embodiment makes the alkalimetal ion in liquefied ammonia insert gradually lamellar compound by step 3 by the vibration silica tube, and the time of the silica tube that generally vibrates is 20min to 1h.Step 4 puts at lamellar compound the generation that the deionized water ultrasonic procedure can be observed bubble.It is in order to remove large-size particle that step 5 is put into whizzer centrifugal.
The general formula of the hydrotalcite in the present embodiment lamellar compound is [Mg
1-xm
x iII(OH)
2] [A
x/n] mH
2o, wherein M
iIIfor ionic radius and the approaching 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: what present embodiment was different from embodiment one is that the described alkali-metal purity of step 1 is not less than 99.9%.Other step and parameter are identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one or two is that the purity of the described lamellar compound of step 1 is not less than 99.9%.Other step and parameter are identical with embodiment one or two.
Embodiment four: what present embodiment was different from one of embodiment one to three is that step 1 is that 1 ︰ 2 takes basic metal and lamellar compound in molar ratio under the environment of protection of inert gas.Other step and parameter are identical with one of embodiment one to three.
Embodiment five: present embodiment is different from one of embodiment one to four is that the type of cooling of the described cooling silica tube of step 2 is to adopt cooled with liquid nitrogen or adopt the mixture of ice and water of ethanol and water cooling.Other step and parameter are identical with one of embodiment one to four.
Embodiment six: present embodiment is different from one of embodiment one to five be step 5 described to put into whizzer centrifugal, wherein centrifugal speed is 3000r/min～15000r/min.Other step and parameter are identical with one of embodiment one to five.
Embodiment mono-: the method that the present embodiment utilizes liquefied ammonia/alkali metal soln to prepare the two-dimensional nano material follows these steps to realize:
One, take the powdered graphite of 0.005mol metallic lithium and 0.01mol in the glove box of argon shield, 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 the cooled with liquid nitrogen silica tube, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, the vibration silica tube continues coolingly in the process of vibration silica tube to silica tube, vibrates and takes off to the blueness of liquid ammonia solution, and then at room temperature vaporize liquefied ammonia extraction obtain the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained is put 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 to whizzer centrifugal with the speed of 4000r/min, then in the supernatant liquid after centrifugal, collect and obtain the two-dimensional nano material.
After the present embodiment step 3 vibration 30min, the blueness of liquid ammonia solution is taken off.
The two-dimensional nano material that the present embodiment obtains is the two-dimensional nano Graphene.
Embodiment bis-: the method that the present embodiment utilizes liquefied ammonia/alkali metal soln to prepare the two-dimensional nano material follows these steps to realize:
One, take the molybdenum disulfide powder of 0.005mol metallic lithium and 0.01mol in the glove box of argon shield, 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 the cooled with liquid nitrogen silica tube, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, the vibration silica tube continues coolingly in the process of vibration silica tube to silica tube, vibrates and takes off to the blueness of liquid ammonia solution, and then at room temperature vaporize liquefied ammonia extraction obtain the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained is put 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 to whizzer centrifugal with the speed of 4000r/min, then in the supernatant liquid after centrifugal, collect and obtain the two-dimensional nano material.
After the present embodiment step 3 vibration 30min, the blueness of liquid ammonia solution is taken off.
The two-dimensional nano material 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 tri-: the method that the present embodiment utilizes liquefied ammonia/alkali metal soln to prepare the two-dimensional nano material follows these steps to realize:
One, take the tungsten disulfide powder of 0.005mol metallic lithium and 0.01mol in the glove box of argon shield, 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 the cooled with liquid nitrogen silica tube, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, the vibration silica tube continues coolingly in the process of vibration silica tube to silica tube, vibrates and takes off to the blueness of liquid ammonia solution, and then at room temperature vaporize liquefied ammonia extraction obtain the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained is put 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 to whizzer centrifugal with the speed of 4000r/min, then in the supernatant liquid after centrifugal, collect and obtain the two-dimensional nano material.
After the present embodiment step 3 vibration 30min, the blueness of liquid ammonia solution is taken off.
The two-dimensional nano material 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 tetra-: the method that the present embodiment utilizes liquefied ammonia/alkali metal soln to prepare the two-dimensional nano material follows these steps to realize:
One, take the titanium disulfide powder of 0.005mol metallic lithium and 0.01mol in the glove box of argon shield, 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 the cooled with liquid nitrogen silica tube, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, the vibration silica tube continues coolingly in the process of vibration silica tube to silica tube, vibrates and takes off to the blueness of liquid ammonia solution, and then at room temperature vaporize liquefied ammonia extraction obtain the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained is put 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 to whizzer centrifugal with the speed of 4000r/min, then in the supernatant liquid after centrifugal, collect and obtain the two-dimensional nano material.
After the present embodiment step 3 vibration 30min, the blueness of liquid ammonia solution is taken off.
The two-dimensional nano material that the present embodiment obtains is the 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 the two-dimensional nano material follows these steps to realize:
One, take the two tellurium molybdenum powder of 0.005mol metallic lithium and 0.01mol in the glove box of argon shield, 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 the cooled with liquid nitrogen silica tube, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, the vibration silica tube continues coolingly in the process of vibration silica tube to silica tube, vibrates and takes off to the blueness of liquid ammonia solution, and then at room temperature vaporize liquefied ammonia extraction obtain the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained is put 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 to whizzer centrifugal with the speed of 4000r/min, then in the supernatant liquid after centrifugal, collect and obtain the two-dimensional nano material.
After the present embodiment step 3 vibration 30min, the blueness of liquid ammonia solution is taken off.
The two-dimensional nano material that the present embodiment obtains is two tellurium molybdenum nanometer sheet.
Embodiment six: the method that the present embodiment utilizes liquefied ammonia/alkali metal soln to prepare the two-dimensional nano material follows these steps to realize:
One, take the two selenizing molybdenum powder of 0.005mol metallic lithium and 0.01mol in the glove box of argon shield, 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 the cooled with liquid nitrogen silica tube, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, the vibration silica tube continues coolingly in the process of vibration silica tube to silica tube, vibrates and takes off to the blueness of liquid ammonia solution, and then at room temperature vaporize liquefied ammonia extraction obtain the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained is put 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 to whizzer centrifugal with the speed of 4000r/min, then in the supernatant liquid after centrifugal, collect and obtain the two-dimensional nano material.
After the present embodiment step 3 vibration 30min, the blueness of liquid ammonia solution is taken off.
The two-dimensional nano material 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 the two-dimensional nano material follows these steps to realize:
One, take the two selenizing tungsten powders of 0.005mol metallic lithium and 0.01mol in the glove box of argon shield, 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 the cooled with liquid nitrogen silica tube, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, the vibration silica tube continues coolingly in the process of vibration silica tube to silica tube, vibrates and takes off to the blueness of liquid ammonia solution, and then at room temperature vaporize liquefied ammonia extraction obtain the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained is put 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 to whizzer centrifugal with the speed of 4000r/min, then in the supernatant liquid after centrifugal, collect and obtain the two-dimensional nano material.
After the present embodiment step 3 vibration 30min, the blueness of liquid ammonia solution is taken off.
The two-dimensional nano material that the present embodiment obtains is two selenizing tungsten nanometer sheet.
Embodiment eight: the method that the present embodiment utilizes liquefied ammonia/alkali metal soln to prepare the two-dimensional nano material follows these steps to realize:
One, take the graphite-phase carbonitride powder of 0.005mol metallic lithium and 0.01mol in the glove box of argon shield, 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 the cooled with liquid nitrogen silica tube, basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, the vibration silica tube continues coolingly in the process of vibration silica tube to silica tube, vibrates and takes off to the blueness of liquid ammonia solution, and then at room temperature vaporize liquefied ammonia extraction obtain the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained is put 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 to whizzer centrifugal with the speed of 4000r/min, then in the supernatant liquid after centrifugal, collect and obtain the two-dimensional nano material.
After the present embodiment step 3 vibration 30min, the blueness of liquid ammonia solution is taken off.
The two-dimensional nano material that the present embodiment obtains is graphite-phase azotized carbon nano 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%.
Show by above embodiment, utilize the basic metal be dissolved in liquefied ammonia to carry out intercalation to lamellar compound, and by the compound after intercalation in deionized water for ultrasonic, can effectively realize the peeling off of lamellar compound prepared to ultra-thin two-dimensional nano material.
Claims (6)
1. a method of utilizing liquefied ammonia/alkali metal soln to prepare the two-dimensional nano material is characterized in that the method for utilizing liquefied ammonia/alkali metal soln to prepare the two-dimensional nano material 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 cooling silica tube liquefies to the ammonia in pipe, and basic metal is dissolved in liquefied ammonia makes liquid ammonia solution present blueness;
Three, the vibration silica tube continues coolingly in the process of vibration silica tube to silica tube, vibrates and takes off to the blueness of liquid ammonia solution, and then at room temperature vaporize liquefied ammonia extraction obtain the lamellar compound after intercalation;
Four, the lamellar compound after intercalation step 3 obtained is put 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 to whizzer centrifugal, then in the supernatant liquid after centrifugal, collect and obtain the two-dimensional nano material;
Wherein the described basic metal of step 1 is lithium, sodium or potassium;
Described lamellar compound is graphite, Vanadium Pentoxide in FLAKES, molybdic oxide, hexagonal boron nitride, metal dithionite compound 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, houghite, transition metal oxide YO
2(wherein Y=Ti, V, Cr, Mn, Fe, Co or Ni), graphite-phase carbonitride, montmorillonite, saponite, vermiculite or rhombspar.
2. a kind of method of utilizing liquefied ammonia/alkali metal soln to prepare the two-dimensional nano material according to claim 1, is characterized in that the described alkali-metal purity of step 1 is not less than 99.9%.
3. a kind of method of utilizing liquefied ammonia/alkali metal soln to prepare the two-dimensional nano material according to claim 1, is characterized in that the purity of the described lamellar compound of step 1 is not less than 99.9%.
4. a kind of method of utilizing liquefied ammonia/alkali metal soln to prepare the two-dimensional nano material according to claim 1, is characterized in that step 1 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 of utilizing liquefied ammonia/alkali metal soln to prepare the two-dimensional nano material according to claim 1, the type of cooling that it is characterized in that the described cooling silica tube of step 2 is to adopt cooled with liquid nitrogen or adopt the mixture of ice and water of ethanol and water cooling.
6. a kind of method of utilizing liquefied ammonia/alkali metal soln to prepare the two-dimensional nano material according to claim 1, it is characterized in that step 5, described to put into whizzer centrifugal, and wherein centrifugal speed is 3000r/min～15000r/min.
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| 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 |
| CN110346430A (en) * | 2019-06-17 | 2019-10-18 | 福建师范大学 | A kind of Na+Adulterate g-C3N4Composite material, electrochemical sensor and preparation method thereof, purposes |
| 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 |
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