CN104402053A - Preparation method for graphene-like two-dimension nanosheet - Google Patents
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Abstract
The invention relates to a novel preparation method for a graphene-like two-dimension nanosheet, and belongs to the technical field of nanometer materials. A layered material powder is taken as a raw material in the method, and the method comprises the following steps: (1) adding a to-be peeled layered material in an anhydrous dispersing solvent, and stirring uniformly to obtain a dispersion solution of the material; (2) adding an alkali metal into the above dispersion solution, and performing rapid stirring or shearing at 10 DEG C-80 DEG C to obtain a crude product; and (3) using the above solvent to wash the obtained crude product, dispersing the washing product in water, then performing ultrasonic dispersing on the obtained dispersion solution for 5-60 min, and using water to wash the product subjected to ultrasonic processing to have the pH value of 6-8, so as to obtain the graphene-like two-dimension nanosheet. The method has the characteristics of high yield, simple preparation technology, low cost, easiness for large-scale production, and the like.
Description
Technical field
The present invention relates to the novel processing step of a kind Graphene two-dimensional nano sheet, belong to technical field of nano material.
Background technology
In recent years, the two-dimensional layer material that a class is novel---class Graphene two-dimension nano materials, causes the extensive concern of the various fields researchists such as physics, chemistry, material, electronics, wherein with class Graphene transient metal chalcogenide compound (MoS
2, WS
2, TiS
2, MoSe
2, WSe
2deng) and hexagonal boron nitride (h-BN) representatively.Because class Graphene two-dimension nano materials has unique structure and interfacial property and high specific surface area, therefore illustrate very large application potential in fields such as lubricant, photoelectricity, catalysis, chemistry and bio-sensing, solar cell and energy storage.Such as, class Graphene MoS
2may be used for electrode material of lithium battery, its nano-lamellar structure is applicable to lithium ion rapid diffusion, and large exposed surface can provide more lithium ion to insert passage; Class Graphene MoS
2there is regulatable band gap, have bright application prospect at field of photoelectric devices; Class Graphene MoS
2there is the two-dimensional layered structure of nanoscale, can also be used to manufacture efficient semiconductor electronic chip, will be widely used in nano-electric devices field of future generation.Class Graphene two-dimension nano materials has the lateral dimension of atom or other thickness of molecular level and submicron or micron level, can obtain by peeling off its corresponding stratified material, such as can stratiform h-BN, MoS
2, WS
2etc. peeling off into individual layer two-dimensional nano sheet, because there is strong chemical bond in its layer, and there is multiple more weak model ylid bloom action power, hydrogen bond and electrostatic interactions in interlayer.The many stratified material delamination technology of development in recent years, investigator utilizes micromechanics stripping method, ion insertion stripping method etc. to be peeled off into individual layer class grapheme two-dimension material.Micromechanics stripping method is by the mode such as high speed shear or high-power ultrasonic among some specific solvents, realizes the method for stripping in the solution, but this mode often productive rate is very low.Ion insertion stripping method can be peeled off by controlling Electrochemical lithiation ion process implementation, but this method complex process, cost is high, high to preparation environmental requirement, is not suitable for large-scale production.Therefore development technology is simple, and productive rate is high, and the preparation method being applicable to the class Graphene two-dimensional nano sheet of scale operation is extremely important.
Summary of the invention
The object of the invention is the preparation method of proposition one kind Graphene two-dimensional nano sheet, select specific anhydrous solvent and basic metal (one or more mixtures of lithium, sodium, potassium), to prepare class Graphene two-dimensional nano sheet, and simplify production technique, reduction production cost, with applicable scale operation.
The preparation method of the class Graphene two-dimensional nano sheet that the present invention proposes, comprises the following steps:
(1) join in anhydrous dispersion solvent by stratified material to be stripped, mass volume ratio is: stratified material: anhydrous dispersion solvent=1 gram: (100 milliliters ~ 1000 milliliters), stir and obtain the first dispersion liquid;
(2) basic metal is joined in the first dispersion liquid that step (1) obtains, mass ratio is: basic metal: stratified material=1 gram: (0.25 gram ~ 5 grams), obtain the second dispersion liquid, then at 10 DEG C ~ 80 DEG C, rapid stirring or shearing are carried out to the second dispersion liquid, stirring or shearing rate are 200rpm ~ 20000rpm, stirring or shear time are 6 ~ 120 hours, obtain crude product;
(3) by the crude product of step (2) with the corresponding anhydrous dispersion solvent wash of step (1) 3 ~ 5 times, again the product after washing is dispersed in water, obtain the 3rd dispersion liquid, then the 3rd dispersion liquid is carried out ultrasonic disperse 5 ~ 60 minutes, and the products in water after ultrasonic is washed till pH value is 6-8, obtain class Graphene two-dimensional nano sheet.
In above-mentioned preparation method, described stratified material to be stripped is hexagonal boron nitride (h-BN) or transient metal chalcogenide compound powder.
In above-mentioned preparation method, described anhydrous dispersion solvent is any one in glycol dimethyl ether, ethylene glycol monomethyl ether, liquefied ammonia, ethamine or quadrol.
In above-mentioned preparation method, described basic metal is that one or more in metallic lithium, sodium Metal 99.5 or potassium metal are with the mixture of any ratio.
The preparation method of the class Graphene two-dimensional nano sheet that the present invention proposes, its advantage is:
The inventive method synthesis technique is simple, and with low cost, production efficiency is high, suitability for scale production.Compared with existing stripping means, the inventive method production technique is simple, and production process is without the need to particular surroundings requirement, and easy control of reaction conditions, the two-dimensional nano sheet obtained has that productive rate is high, result is reproducible, be suitable for the advantages such as suitability for industrialized production.Class Graphene two-dimensional nano sheet prepared by the inventive method, can be applied to lubricant, chemistry and bio-sensing, photochemical catalysis, li-ion electrode materials etc., can also prepare polymer composites and graphene composite material as addO-on therapy.The inventive method is suitable for preparation class Graphene transient metal chalcogenide compound nanometer sheet (MoS
2, WS
2, TiS
2, FeS
2, MoSe
2, WSe
2deng) and hexagonal boron nitride nanosheet, raw materials used is block or the powder of its corresponding stratified material, such as MoS
2nanometer sheet can pass through stratiform MoS
2the stripping of powder obtains.
Accompanying drawing explanation
Fig. 1 is MoS prepared by the embodiment 1 of the inventive method
2the photo that nanometer sheet is disperseed in water.
Fig. 2 is MoS prepared by the embodiment 1 of the inventive method
2the TEM figure of nanometer sheet.
Fig. 3 is MoS prepared by the embodiment 1 of the inventive method
2the HRTEM figure of nanometer sheet.
Fig. 4 is MoS prepared by the embodiment 1 of the inventive method
2the diffractogram of nanometer sheet.
Fig. 5 is MoS prepared by the embodiment 1 of the inventive method
2the AFM figure of nanometer sheet.
Fig. 6 is MoS prepared by the embodiment 1 of the inventive method
2the XRD figure of nanometer sheet.
Fig. 7 is WS prepared by the embodiment 2 of the inventive method
2the photo that nanometer sheet is disperseed in water.
Fig. 8 is WS prepared by the embodiment 2 of the inventive method
2the TEM figure of nanometer sheet.
Fig. 9 is the photo that the BN nanometer sheet of embodiment 3 preparation of the inventive method is disperseed in water.
Figure 10 is the TEM figure of BN nanometer sheet prepared by the embodiment 3 of the inventive method.
Embodiment
The preparation method of the class Graphene two-dimensional nano sheet that the present invention proposes, comprises the following steps:
(1) join in anhydrous dispersion solvent by stratified material to be stripped, mass volume ratio is: stratified material: anhydrous dispersion solvent=1 gram: (100 milliliters ~ 1000 milliliters), stir and obtain the first dispersion liquid;
(2) basic metal is joined in the first dispersion liquid that step (1) obtains, mass ratio is: basic metal: stratified material=1 gram: (0.25 gram ~ 5 grams), obtain the second dispersion liquid, then at 10 DEG C ~ 80 DEG C, rapid stirring or shearing are carried out to the second dispersion liquid, stirring or shearing rate are 200rpm ~ 20000rpm, stirring or shear time are 6 ~ 120 hours, obtain crude product;
(3) by the crude product of step (2) with the corresponding anhydrous dispersion solvent wash of step (1) 3 ~ 5 times, again the product after washing is dispersed in water, obtain the 3rd dispersion liquid, then the 3rd dispersion liquid is carried out ultrasonic disperse 5 ~ 60 minutes, and the products in water after ultrasonic is washed till pH value is 6-8, obtain class Graphene two-dimensional nano sheet.
Stratified material to be stripped in above-mentioned preparation method is hexagonal boron nitride (h-BN) or transient metal chalcogenide compound powder.
Anhydrous dispersion solvent in above-mentioned preparation method is any one in glycol dimethyl ether, ethylene glycol monomethyl ether, liquefied ammonia, ethamine or quadrol.
Basic metal in aforesaid method is that one or more in metallic lithium, sodium Metal 99.5 or potassium metal are with the mixture of any ratio.
Preparation method of the present invention, by solvent rapid stirring together with basic metal (one or more mixtures of lithium, sodium, potassium), alkali metal atom and ion is discharged by solvent and alkali-metal effect, and then be intercalation into the interlayer of the stratified material such as boron nitride or transient metal chalcogenide compound, destroy its laminate structure, and under the shearing action of solvent, realize the stripping of lamella, the class Graphene two-dimensional nano sheet of high yield can be obtained further by ultrasonic effect simultaneously.
Introduce the embodiment of the inventive method below:
Embodiment one:
(1) with 1 gram of MoS2 powder for raw material, join in 200 milliliters of glycol dimethyl ethers, stir and obtain its dispersion liquid;
(2) respectively 1.2 grams of sodium Metal 99.5s and 1.5 grams of potassium metals are cut into small pieces in glycol dimethyl ether, and join in the dispersion liquid that step (1) obtains together, then at 25 DEG C, rapid stirring is carried out to described dispersion liquid, stir speed (S.S.) is 1000rpm, churning time is 48 hours, obtains crude product;
(3) by the crude product of step (2) above-mentioned solvent wash 5 times, then the product after washing is dispersed in water, then gained dispersion liquid is carried out ultrasonic disperse 15min, and the products in water after ultrasonic is washed till pH value 6-8.
Figure 1 shows that MoS prepared by the embodiment 1 of the inventive method
2the photo that nanometer sheet is disperseed in water.Fig. 2 is MoS prepared by the embodiment 1 of the inventive method
2the TEM figure of nanometer sheet.Fig. 3 is MoS prepared by the embodiment 1 of the inventive method
2the HRTEM figure of nanometer sheet.Fig. 4 is MoS prepared by the embodiment 1 of the inventive method
2the diffractogram of nanometer sheet.Fig. 5 is MoS prepared by the embodiment 1 of the inventive method
2the AFM figure of nanometer sheet, can find out that its number of plies only has 1-2 layer.Class Graphene MoS prepared by the embodiment 1 that Fig. 6 sets forth the inventive method
2nanometer sheet with stratiform MoS
2the XRD figure of raw material, the MoS after can stripping being found out
2nanometer sheet XRD peak disappears, and proves successfully to prepare MoS
2nanometer sheet.
Embodiment two:
(1) with 1 gram of WS
2powder is raw material, joins in 200 milliliters of glycol dimethyl ethers, stirs and obtain its dispersion liquid;
(2) respectively 1.2 grams of sodium Metal 99.5s and 1.5 grams of potassium metals are cut into small pieces in glycol dimethyl ether, and join in the dispersion liquid that step (1) obtains together, then at 25 DEG C, rapid stirring is carried out to described dispersion liquid, stir speed (S.S.) is 1000rpm, churning time is 48 hours, obtains crude product;
(3) by the crude product of step (2) above-mentioned solvent wash 5 times, then the product after washing is dispersed in water, then gained dispersion liquid is carried out ultrasonic disperse 15min, and the products in water after ultrasonic is washed till pH value 6-8.
WS prepared by the embodiment 2 being illustrated in figure 7 the inventive method
2the photo that nanometer sheet is disperseed in water.Fig. 8 is WS prepared by the embodiment 2 of the inventive method
2the TEM figure of nanometer sheet.
Embodiment three:
(1) with 1 gram of hexagonal boron nitride powder for raw material, join in 200 milliliters of glycol dimethyl ethers, stir and obtain its dispersion liquid;
(2) respectively 1.2 grams of sodium Metal 99.5s and 1.5 grams of potassium metals are cut into small pieces in glycol dimethyl ether, and join in the dispersion liquid that step (1) obtains together, then at 25 DEG C, rapid stirring is carried out to described dispersion liquid, stir speed (S.S.) is 1000rpm, churning time is 48 hours, obtains crude product;
(3) by the crude product of step (2) above-mentioned solvent wash 5 times, then the product after washing is dispersed in water, then gained dispersion liquid is carried out ultrasonic disperse 15min, and the products in water after ultrasonic is washed till pH value 6-8.
The photo that BN nanometer sheet prepared by the embodiment 3 being illustrated in figure 9 the inventive method is disperseed in water.Figure 10 is the TEM figure of BN nanometer sheet prepared by the embodiment 3 of the inventive method.
Embodiment four:
(1) with 1 gram of MoS
2powder is raw material, joins in 200 milliliters of glycol dimethyl ethers, stirs and obtain its dispersion liquid;
(2) 2 grams of sodium Metal 99.5s are cut into small pieces in glycol dimethyl ether, and join in the dispersion liquid that step (1) obtains, then at 25 DEG C, carry out rapid stirring to described dispersion liquid, stir speed (S.S.) is 1000rpm, churning time is 72 hours, obtains crude product;
(3) by the crude product of step (2) above-mentioned solvent wash 5 times, then the product after washing is dispersed in water, then gained dispersion liquid is carried out ultrasonic disperse 15min, and the products in water after ultrasonic is washed till pH value 6-8.
Embodiment five:
(1) with 1 gram of MoS
2powder is raw material, joins in 200 milliliters of glycol dimethyl ethers, stirs and obtain its dispersion liquid;
(2) 2 grams of potassium metals are cut into small pieces in glycol dimethyl ether, and join in the dispersion liquid that step (1) obtains, then at 25 DEG C, carry out rapid stirring to described dispersion liquid, stir speed (S.S.) is 1000rpm, churning time is 72 hours, obtains crude product;
(3) by the crude product of step (2) above-mentioned solvent wash 5 times, then the product after washing is dispersed in water, then gained dispersion liquid is carried out ultrasonic disperse 15min, and the products in water after ultrasonic is washed till pH value 6-8.
Embodiment six:
(1) with 1 gram of WS
2powder is raw material, joins in 200 milliliters of glycol dimethyl ethers, stirs and obtain its dispersion liquid;
(2) 2 grams of sodium Metal 99.5s are cut into small pieces in glycol dimethyl ether, and join in the dispersion liquid that step (1) obtains, then at 30 DEG C, carry out rapid stirring to described dispersion liquid, stir speed (S.S.) is 1000rpm, churning time is 72 hours, obtains crude product;
(3) by the crude product of step (2) above-mentioned solvent wash 5 times, then the product after washing is dispersed in water, then gained dispersion liquid is carried out ultrasonic disperse 15min, and the products in water after ultrasonic is washed till pH value 6-8.
Embodiment seven:
(1) with 1 gram of WS
2powder is raw material, joins in 200 milliliters of glycol dimethyl ethers, stirs and obtain its dispersion liquid;
(2) 2 grams of potassium metals are cut into small pieces in glycol dimethyl ether, and join in the dispersion liquid that step (1) obtains, then at 30 DEG C, carry out rapid stirring to described dispersion liquid, stir speed (S.S.) is 1000rpm, churning time is 72 hours, obtains crude product;
(3) by the crude product of step (2) above-mentioned solvent wash 5 times, then the product after washing is dispersed in water, then gained dispersion liquid is carried out ultrasonic disperse 15min, and the products in water after ultrasonic is washed till pH value 6-8.
Embodiment eight:
(1) with 1 gram of hexagonal boron nitride powder for raw material, join in 200 milliliters of glycol dimethyl ethers, stir and obtain its dispersion liquid;
(2) 2 grams of potassium metals are cut into small pieces in glycol dimethyl ether, and join in the dispersion liquid that step (1) obtains, then at 25 DEG C, carry out rapid stirring to described dispersion liquid, stir speed (S.S.) is 1000rpm, churning time is 72 hours, obtains crude product;
(3) by the crude product of step (2) above-mentioned solvent wash 5 times, then the product after washing is dispersed in water, then gained dispersion liquid is carried out ultrasonic disperse 25min, and the products in water after ultrasonic is washed till pH value 6-8.
Embodiment nine:
(1) with 1 gram of MoS
2powder is raw material, joins in 200 milliliters of liquefied ammonia, stirs and obtain its dispersion liquid;
(2) respectively 1.2 grams of sodium Metal 99.5s and 1.5 grams of potassium metals are cut into small pieces, and join together in the dispersion liquid that step (1) obtains, then at 25 DEG C, carry out rapid stirring to described dispersion liquid, stir speed (S.S.) is 700rpm, churning time is 240 hours, obtains crude product;
(3) by the crude product of step (2) above-mentioned solvent wash 5 times, then the product after washing is dispersed in water, then gained dispersion liquid is carried out ultrasonic disperse 30min, and the products in water after ultrasonic is washed till pH value 6-8.
Embodiment ten:
(1) with 1 gram of MoS
2powder is raw material, joins in 200 milliliters of glycol dimethyl ethers, stirs and obtain its dispersion liquid;
(2) respectively 1.2 grams of sodium Metal 99.5s and 1.5 grams of potassium metals are cut into small pieces in glycol dimethyl ether, and join in the dispersion liquid that step (1) obtains together, then at 65 DEG C, rapid stirring is carried out to described dispersion liquid, stir speed (S.S.) is 1000rpm, churning time is 48 hours, obtains crude product;
(3) by the crude product of step (2) above-mentioned solvent wash 5 times, then the product after washing is dispersed in water, then gained dispersion liquid is carried out ultrasonic disperse 30min, and the products in water after ultrasonic is washed till pH value 6-8.
Embodiment 11:
(1) with 1 gram of MoS
2powder is raw material, joins in 200 milliliters of glycol dimethyl ethers, stirs and obtain its dispersion liquid;
(2) respectively 1.8 grams of sodium Metal 99.5s and 3.2 grams of potassium metals are cut into small pieces in glycol dimethyl ether, and join in the dispersion liquid that step (1) obtains together, then at 25 DEG C, rapid stirring is carried out to described dispersion liquid, stir speed (S.S.) is 1000rpm, churning time is 72 hours, obtains crude product;
(3) by the crude product of step (2) above-mentioned solvent wash 5 times, then the product after washing is dispersed in water, then gained dispersion liquid is carried out ultrasonic disperse 30min, and the products in water after ultrasonic is washed till pH value 6-8.
Embodiment 11:
(1) with 1 gram of MoS2 powder for raw material, join in 200 milliliters of glycol dimethyl ethers, stir and obtain its dispersion liquid;
(2) respectively 1.2 grams of sodium Metal 99.5s and 1.5 grams of potassium metals are cut into small pieces in glycol dimethyl ether, and join in the dispersion liquid that step (1) obtains together, then at 10 DEG C, rapid stirring is carried out to described dispersion liquid, stir speed (S.S.) is 5000rpm, churning time is 48 hours, obtains crude product;
(3) by the crude product of step (2) above-mentioned solvent wash 5 times, then the product after washing is dispersed in water, then gained dispersion liquid is carried out ultrasonic disperse 5min, and the products in water after ultrasonic is washed till pH value 6-8.
Embodiment 12:
(1) with 1 gram of MoS
2powder is raw material, joins in 200 milliliters of liquefied ammonia, stirs and obtain its dispersion liquid;
(2) respectively 1.2 grams of sodium Metal 99.5s and 1.5 grams of potassium metals are cut into small pieces, and join together in the dispersion liquid that step (1) obtains, then at 25 DEG C, carry out THE ADIABATIC SHEAR IN to described dispersion liquid, shearing rate is 20000rpm, churning time is 5 hours, obtains crude product;
(3) by the crude product of step (2) above-mentioned solvent wash 5 times, then the product after washing is dispersed in water, then gained dispersion liquid is carried out ultrasonic disperse 5min, and the products in water after ultrasonic is washed till pH value 6-8.
Embodiment 13:
(1) with 1 gram of WS
2powder is raw material, joins in 200 milliliters of liquefied ammonia, stirs and obtain its dispersion liquid;
(2) respectively 1 gram of sodium Metal 99.5 and 1.2 grams of potassium metals are cut into small pieces, and join together in the dispersion liquid that step (1) obtains, then at 10 DEG C, carry out THE ADIABATIC SHEAR IN to described dispersion liquid, shearing rate is 15000rpm, churning time is 5 hours, obtains crude product;
(3) by the crude product of step (2) above-mentioned solvent wash 5 times, then the product after washing is dispersed in water, then gained dispersion liquid is carried out ultrasonic disperse 10min, and the products in water after ultrasonic is washed till pH value 6-8.
Embodiment 14:
(1) with 1 gram of hexagonal boron nitride powder for raw material, join in 300 milliliters of liquefied ammonia, stir and obtain its dispersion liquid;
(2) respectively 1.2 grams of sodium Metal 99.5s and 1.5 grams of potassium metals are cut into small pieces, and join together in the dispersion liquid that step (1) obtains, then at 15 DEG C, carry out THE ADIABATIC SHEAR IN to described dispersion liquid, shearing rate is 10000rpm, churning time is 5 hours, obtains crude product;
(3) by the crude product of step (2) above-mentioned solvent wash 5 times, then the product after washing is dispersed in water, then gained dispersion liquid is carried out ultrasonic disperse 10min, and the products in water after ultrasonic is washed till pH value 6-8.
Claims (4)
1. the preparation method of a kind Graphene two-dimensional nano sheet, is characterized in that this preparation method comprises the following steps:
(1) join in anhydrous dispersion solvent by stratified material to be stripped, mass volume ratio is: stratified material: anhydrous dispersion solvent=1 gram: (100 milliliters ~ 1000 milliliters), stir and obtain the first dispersion liquid;
(2) basic metal is joined in the first dispersion liquid that step (1) obtains, mass ratio is: basic metal: stratified material=1 gram: (0.25 gram ~ 5 grams), obtain the second dispersion liquid, then at 10 DEG C ~ 80 DEG C, rapid stirring or shearing are carried out to the second dispersion liquid, stirring or shearing rate are 200rpm ~ 20000rpm, stirring or shear time are 6 ~ 120 hours, obtain crude product;
(3) by the crude product of step (2) with the corresponding anhydrous dispersion solvent wash of step (1) 3 ~ 5 times, again the product after washing is dispersed in water, obtain the 3rd dispersion liquid, then the 3rd dispersion liquid is carried out ultrasonic disperse 5 ~ 60 minutes, and the products in water after ultrasonic is washed till pH value is 6-8, obtain class Graphene two-dimensional nano sheet.
2. preparation method as claimed in claim 1, is characterized in that wherein said stratified material to be stripped is hexagonal boron nitride or transient metal chalcogenide compound powder.
3. preparation method as claimed in claim 1, is characterized in that wherein said anhydrous dispersion solvent is any one in glycol dimethyl ether, ethylene glycol monomethyl ether, liquefied ammonia, ethamine or quadrol.
4. preparation method as claimed in claim 1, is characterized in that the wherein said basic metal described in step (2) is that one or more in metallic lithium, sodium Metal 99.5 or potassium metal are with the mixture of any ratio.
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101898766A (en) * | 2009-05-25 | 2010-12-01 | 北京化工大学 | Method for efficiently-stripped laminar inorganic material |
CN103496692A (en) * | 2013-09-17 | 2014-01-08 | 哈尔滨工业大学 | Method for preparing two-dimensional nanomaterial by utilizing liquid ammonia/alkali metal solution |
CN103641172A (en) * | 2013-12-19 | 2014-03-19 | 中国科学院上海硅酸盐研究所 | Method for preparing nanometer layered molybdenum disulfide |
-
2014
- 2014-11-04 CN CN201410612347.1A patent/CN104402053B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101898766A (en) * | 2009-05-25 | 2010-12-01 | 北京化工大学 | Method for efficiently-stripped laminar inorganic material |
CN103496692A (en) * | 2013-09-17 | 2014-01-08 | 哈尔滨工业大学 | Method for preparing two-dimensional nanomaterial by utilizing liquid ammonia/alkali metal solution |
CN103641172A (en) * | 2013-12-19 | 2014-03-19 | 中国科学院上海硅酸盐研究所 | Method for preparing nanometer layered molybdenum disulfide |
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