CN107416783B - Method for passivating black phosphorus nano material - Google Patents
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Abstract
The invention discloses a method for passivating black phosphorus nano material by adjusting Zn (CH)3COO)2The proportion of KOH and black phosphorus quantum dots controls the appearance of a composite structure of ZnO nanocrystals and black phosphorus nano materials, and because the conduction band of the black phosphorus is positioned below the conduction band of the ZnO, electrons of the ZnO can be naturally transferred into the black phosphorus by the energy band structure, and the excessive electrons in the black phosphorus can slow down the oxidation of the black phosphorus, thereby achieving the effect of passivating the surface of the black phosphorus. The method for passivating the black phosphorus nano material provided by the invention is simple and easy to implement and low in cost, and the prepared ZnO nanocrystal and black phosphorus nano material composite structure can greatly improve the stability of the black phosphorus nano material.
Description
Technical Field
The invention relates to the field of black phosphorus nano materials, in particular to a method for passivating a black phosphorus nano material.
Background
Black phosphorus, an important van DE Wales two-dimensional material, has a direct energy band structure, and the band gap can be adjusted from 0.3eV to 2eV along with the layer thickness. The black phosphorus material has the carrier mobility as high as 1000 cm at room temperature2V-1s-1The method has certain advantages in the application aspect of (optical) electronic devices, and can be used for manufacturing sensors, field effect transistors, photoelectric detectors, capacitors and the like. The black phosphorus also has a unique in-plane anisotropic structure and shows unique angle-dependent properties such as angle-dependent electrical conduction and polarization optical characteristics, and opens up a new way for the application of the black phosphorus. However, black Phosphorus exposed to the environment forms bubbles on the surface due to oxygen and water vapor present in the air and photo-oxidation in the environment, and is rapidly degraded to form phosphoric acid (Bridgman, P.W. two New Modifications of phosphorous, Collected Experimental Papers; Harvard university Press: Boston, 1964; p 712.), which seriously affects the preparation and processing of black Phosphorus. Thus, the black phosphorus is effectively protectedEspecially, the protection of the black phosphorus nanometer material is very necessary. In the current literature reports, the main methods for enhancing the stability of black phosphorus are divided into two types: (1) reducing the exposure of black phosphorus in air, such as surface organofunctional group modification (Elisa Passagia, ORCID logo, France sca Cicogna, ect. RSC.Adv.2016,26, 53777-; (2) the formation of P-C bonds or P-O-C bonds on the black phosphorus surface passivates the black phosphorus surface (Z. Sofer, J. Luxa, D. Bou š a, D. Sedmidbsk ý, ect. Angew. chem. 10.1002). Although both of the existing methods can play a role in passivating black phosphorus to some extent, the implementation process is complex and the cost is high.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a method for passivating black phosphorus nano-materials, and aims to solve the problems of complex process, poor passivation effect and high cost of the conventional method for passivating black phosphorus.
The technical scheme of the invention is as follows:
a method of passivating black phosphorus nanomaterials, comprising the steps of:
A. grinding the black phosphorus blocks, dispersing the ground black phosphorus blocks into an N-methyl pyrrolidone solution, and performing ultrasonic treatment for 5-8 hours to obtain black phosphorus mixed solutions with different sizes;
B. carrying out step-by-step centrifugal treatment on the black phosphorus mixed solution by using a centrifugal force with a preset gradient to obtain a black phosphorus quantum dot colloidal solution;
C. adding Zn (CH) into the black phosphorus quantum dot colloidal solution under the inert gas atmosphere3COO)2Refluxing in water bath at 50-70 deg.C for 60-120min to obtain acetate precursor solution;
D. adding a pre-prepared N-methylpyrrolidone saturated solution of KOH into the acetate precursor solution, and reacting at the constant temperature of 50-60 ℃ for 120-210min to obtain a precipitate with a composite structure of ZnO nanocrystals and the black phosphorus nano material, thereby realizing the passivation of the black phosphorus nano material.
The above-mentionedThe method for passivating black phosphorus nanomaterial of (1), wherein the Zn (CH)3COO)2The mol ratio of the black phosphorus quantum dots to the black phosphorus quantum dots is 1:0.1-1: 0.5.
The method for passivating the black phosphorus nano material comprises the following steps of:
dissolving KOH in N-methylpyrrolidone solution, stirring for 30-60min at 50-70 ℃, and filtering to obtain the N-methylpyrrolidone saturated solution of KOH.
The method for passivating the black phosphorus nano material, wherein Zn (CH)3COO)2The molar ratio to KOH is from 1:1.67 to 1: 2.
The method for passivating the black phosphorus nanometer material is characterized in that the centrifugal force of the preset gradient is as follows: 70 Xg-20000 Xg, wherein g =9.80m/s2。
The method for passivating the black phosphorus nano material is characterized in that the inert gas is one or more of nitrogen, argon, helium or neon.
The method for passivating the black phosphorus nanometer material further comprises the following steps after the step D:
E. and (3) cooling with cold water to terminate the reaction, and then centrifugally washing with N-methyl pyrrolidone for 3 times to obtain the purified ZnO nanocrystal and black phosphorus nanomaterial composite structure precipitate.
Has the advantages that: the invention provides a method for passivating black phosphorus nano material by regulating Zn (CH)3COO)2The proportion of KOH and black phosphorus quantum dots controls the appearance of a composite structure of ZnO nanocrystals and black phosphorus nano materials, and because the conduction band of the black phosphorus is positioned below the conduction band of the ZnO, electrons of the ZnO can be naturally transferred into the black phosphorus by the energy band structure, and the excessive electrons in the black phosphorus can slow down the oxidation of the black phosphorus, thereby achieving the effect of passivating the surface of the black phosphorus. The method for passivating the black phosphorus nano material provided by the invention is simple and easy to implement and low in cost, and the prepared ZnO nanocrystal and black phosphorus nano material composite structure can greatly improve the stability of the black phosphorus nano material.
Drawings
FIG. 1 is a flow chart of a preferred embodiment of a method for passivating black phosphorus nanomaterials in accordance with the present invention;
FIG. 2 is an electron microscope image of a preferred embodiment of the composite structure of ZnO nanocrystals and black phosphorus nanomaterial prepared in example 1 of the present invention;
FIG. 3 is an EDS mapping chart of oxygen element measured in a composite structure of ZnO nanocrystals and black phosphorus nanomaterial prepared in example 1 of the present invention;
FIG. 4 is an EDS mapping chart of zinc element measured in the composite structure of ZnO nanocrystal and black phosphorus nanomaterial prepared in example 1 of the present invention;
FIG. 5 is an EDS mapping chart of phosphorus element measured in a composite structure of ZnO nanocrystal and black phosphorus nanomaterial prepared in example 1 of the present invention;
FIG. 6 is a Raman spectrum of a composite structure of ZnO nanocrystals and black phosphorus nanomaterial prepared in example 1 of the present invention in comparison with zinc oxide and black phosphorus materials;
FIG. 7 is a Raman spectrum of the composite structure of ZnO nanocrystals and black phosphorus nanomaterial prepared in example 1 of the present invention after UV irradiation for different periods of time compared with that of black phosphorus material;
fig. 8 is a Raman spectrum of the ZnO nanocrystal/black phosphorus nanomaterial composite structure prepared in example 1 of the present invention after exposure to air for 50 days in comparison with the unexposed ZnO nanocrystal/black phosphorus nanomaterial composite structure.
Detailed Description
The invention provides a method for passivating black phosphorus nano-materials, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, fig. 1 is a flow chart of a method for passivating black phosphorus nano-material according to a preferred embodiment of the present invention, as shown in the figure, wherein the method comprises the following steps:
s1, grinding the black phosphorus blocks, dispersing the black phosphorus blocks into an N-methyl pyrrolidone solution, and carrying out ultrasonic treatment for 5-8 hours to obtain black phosphorus mixed solutions with different sizes;
s2, performing step-by-step centrifugal treatment on the black phosphorus mixed solution by using a centrifugal force with a preset gradient to obtain a black phosphorus quantum glue dispersing agent solution;
s3, adding Zn (CH) into the black phosphorus quantum dot colloidal solution under the inert gas atmosphere3COO)2Refluxing in water bath at 50-70 deg.C for 60-120min to obtain acetate precursor solution;
s4, adding a pre-prepared N-methylpyrrolidone saturated solution of KOH into the acetate precursor solution, and reacting at a constant temperature of 50-60 ℃ for 120-210min to obtain a precipitate of a composite structure of ZnO nanocrystals and the black phosphorus nano material, thereby realizing passivation of the black phosphorus nano material.
In particular, the prior art generally improves the stability of black phosphorus by performing organic functional group modification on the surface of black phosphorus to reduce the exposure of black phosphorus in air or passivating the surface of black phosphorus by generating a P-C bond or a P-O-C bond on the surface of black phosphorus; however, the two methods are complex in implementation process and high in cost, and the passivation effect of the black phosphorus is poor, so that the stability of the black phosphorus cannot be remarkably improved.
In order to solve the problems, the invention provides a method for passivating black phosphorus nano material by adding Zn (CH)3COO)2Dissolving the precursor solution in a black phosphorus quantum dot colloidal solution, introducing inert gas into the solution, reacting to obtain an acetate precursor solution, adding an N-methylpyrrolidone saturated solution of KOH into the acetate precursor solution, and reacting to obtain a ZnO nanocrystal and black phosphorus nanomaterial composite structure.
In particular, ZnO is an important II-VI family direct band gap and wide band gap semiconductor material, the band gap at room temperature is 3.37eV, the exciton confinement energy is as high as 60meV, the ZnO can effectively work at room temperature (26 meV) and higher temperature, and the optical gain coefficient (300 cm)-1) Higher than GaN (100 cm)-1) ZnO is rapidly a new international hotspot for researching short-wave (blue and ultraviolet) semiconductor light-emitting device materials after GaN. Because the conduction band of the black phosphorus is positioned below the conduction band of the ZnO, electrons of the ZnO are naturally transferred into the black phosphorus by the band structure, and the excessive electrons in the black phosphorus can slow down the black phosphorusOxidizing to passivate the black phosphorus surface. Therefore, the formation of ZnO coating layer or the formation of composite structure with other materials is an effective way to improve the performance of other nano materials or adjust the properties of other nano materials.
The invention regulates Zn (CH) by regulating3COO)2The proportion of KOH and black phosphorus quantum dots controls the appearance of a composite structure of ZnO nanocrystals and black phosphorus nano materials, and because the conduction band of the black phosphorus is positioned below the conduction band of the ZnO, electrons of the ZnO can be naturally transferred into the black phosphorus by the energy band structure, and the excessive electrons in the black phosphorus can slow down the oxidation of the black phosphorus, thereby achieving the effect of passivating the surface of the black phosphorus. In conclusion, the method for passivating the black phosphorus nano material provided by the invention is simple and easy to implement and has low cost, and the prepared ZnO nanocrystal and black phosphorus nano material composite structure can greatly improve the stability of the black phosphorus nano material.
In the invention, the preparation process of the N-methylpyrrolidone saturated solution of KOH comprises the following steps: dissolving KOH in N-methylpyrrolidone solution, stirring for 30-60min at 50-70 ℃, and filtering to obtain the N-methylpyrrolidone saturated solution of KOH. Further, the Zn (CH)3COO)2The mol ratio of the Zn (CH) to the black phosphorus quantum dots is preferably 1:0.1-1:0.53COO)2The mol ratio of the ZnO nanocrystal to KOH is preferably 1:1.67-1:2, and the prepared ZnO nanocrystal can fully wrap the black phosphorus nanomaterial within the range of the ratio, so that a stable composite structure is formed.
Further, in the present invention, the centrifugal force of the predetermined gradient in step S2 is: 70 Xg-20000 Xg, wherein g =9.80m/s2Specifically, since the black phosphorus material with a larger size is easy to wrap the black phosphorus material with a smaller size, if a one-step centrifugation method is adopted, the black phosphorus material with a smaller size is easy to filter; the invention can obtain enough small-particle black phosphorus nano-materials by gradient centrifugation step by step screening, and preferably can screen the black phosphorus nano-materials with smaller particle size step by centrifugal forces of 70 Xg, 500 Xg, 1000 Xg, 5000 Xg, 10000 Xg and 20000 Xg.
Further, in the step S3, the inert gas is one or more of nitrogen, argon, helium or neon.
Further, in the step S4, a N-methylpyrrolidone saturated solution of KOH prepared in advance is added to the acetate precursor solution, and the mixture reacts at a constant temperature of 50-60 ℃ for 120-210min to obtain a precipitate of a composite structure of ZnO nanocrystals and the black phosphorus nanomaterial, thereby realizing passivation of the black phosphorus nanomaterial.
Specifically, when the temperature is higher than 60 ℃ or the reaction time exceeds 210min, the N-methylpyrrolidone can undergo a ring-opening reaction to cause solvent deterioration, and meanwhile, the ZnO nanocrystal can not uniformly coat the black phosphorus nanomaterial due to overhigh reaction temperature or overlong reaction time, so that the nucleation rate is increased, the particle growth is too fast, and the ZnO nanocrystal coated black phosphorus nanomaterial cannot be obtained; when the temperature is lower than 50 ℃, the crystallization quality of ZnO is influenced, the generated ZnO has more defects, and when the time is lower than 120min, Zn is generated2+Can not be effectively adsorbed on the surface of P atoms, and the coating efficiency is reduced even the coating is unsuccessful. Therefore, the invention preferably performs constant temperature reaction for 120-210min at the temperature of 50-60 ℃ to ensure that Zn is ensured2+The black phosphorus nanometer material is fully and effectively adsorbed on the surface of a P atom, and ZnO nanometer crystals are efficiently generated to coat the black phosphorus nanometer material, so that a composite structure of the ZnO nanometer crystals and the black phosphorus nanometer material is formed, the black phosphorus nanometer material is passivated, and the stability of the black phosphorus nanometer material is improved.
Preferably, in the present invention, after the step S4, the method further includes:
and S5, cooling with cold water to terminate the reaction, and then centrifugally washing with N-methyl pyrrolidone for 3 times to obtain the purified ZnO nanocrystal and black phosphorus nanomaterial composite structure precipitate.
The method for passivating black phosphorus nanomaterial of the present invention is further explained by the following specific examples:
example 1
In this example, the purity specifications of the raw materials used were: zn (CH)3COO)2(99.9 +%), KOH particles (85%), deionized water (R =16.2M Ω), chloroform (chromatographically pure), N-methylpyrrolidone (R99.9%）。
(1) Grinding 5mg of black phosphorus blocks, dispersing the ground black phosphorus blocks in 20ml of N-methyl pyrrolidone solution, and carrying out ultrasonic treatment for 6 hours to obtain mixed solutions of black phosphorus with different layers;
(2) the resulting mixed solution was mixed at a constant gradient of 70 xg, 278 xg, 1112 xg, 2503 xg, 6953 xg, 13628 xg and 17800 xg (g =9.80 m/s)2) The centrifugal force is gradually centrifuged to obtain the black phosphorus quantum glue colloidal solution;
(3) 47.58mg of Zn (CH)3COO)2Dissolving in 10ml of black phosphorus quantum dot colloidal solution, introducing nitrogen into the solution to ensure that the whole reaction is in a nitrogen atmosphere, and simultaneously refluxing in a water bath at 60 ℃ for 60 minutes to obtain Zn (CH)3COO)2Acetate precursor solution of (1);
(4) dissolving 29.12mgKOH in N-methylpyrrolidone solution, stirring for 60 minutes at 60 ℃, and filtering to obtain N-methylpyrrolidone saturated solution of KOH;
(5) adding saturated solution of KOH N-methyl pyrrolidone dropwise to the obtained Zn (CH)3COO)2In the precursor solution, Zn (CH)3COO)2Reacting at the constant temperature of 60 ℃ for 150 minutes to obtain ZnO nanocrystal and black phosphorus nanomaterial composite structure precipitate, wherein the molar ratio of the ZnO nanocrystal to KOH is 1: 1.67;
(6) cooling with ice water to terminate the reaction, and centrifuging and washing with N-methyl pyrrolidone for 3 times to obtain the precipitate with the composite structure of the purified ZnO nanocrystal and the black phosphorus nanomaterial.
The invention performs electron microscope scanning on the composite structure of the ZnO nanocrystal and the black phosphorus nanomaterial prepared in example 1 to obtain an image shown in fig. 2, and simultaneously performs EDS test on the composite structure of the ZnO nanocrystal and the black phosphorus nanomaterial in fig. 2 to obtain the content of oxygen in the scanning area shown in fig. 3, the content of zinc in the scanning area shown in fig. 4, and the content of phosphorus in the scanning area shown in fig. 5.
Further, the Raman signal test was also performed on the ZnO nanocrystal and Black Phosphorus (BP) nanomaterial composite structure prepared in example 1, as shown in fig. 6, pure ZnO nanocrystals and black phosphorus quantum dots had no significant Raman signal, but the black phosphorus Raman signal in the ZnO nanocrystal and black phosphorus nanomaterial composite structure was significantly enhanced, indicating that the stability of black phosphorus was significantly improved.
Furthermore, after the composite structure of the ZnO nanocrystal and the Black Phosphorus (BP) nanomaterial prepared in example 1 is subjected to different treatments, Raman signal detection is performed on the composite structure, and the results are shown in fig. 7 and 8; the comparison shows that the Raman intensity and the normalized intensity of the ZnO-BP composite structure are correspondingly reduced after the ZnO-BP composite structure is exposed in air or irradiated by ultraviolet, and compared with the single BP, the Raman intensity of the ZnO-BP composite structure is far greater than that of the BP, which shows that the stability of the ZnO-BP composite structure is obviously stronger than that of the single black phosphorus material.
In summary, the present invention provides a method for passivating black phosphorus nano-material by adjusting Zn (CH)3COO)2The proportion of the acetate precursor to KOH and black phosphorus controls the appearance of the composite structure of the ZnO nanocrystal and black phosphorus nanomaterial, and because the conduction band of the black phosphorus is positioned below the conduction band of the ZnO, electrons of the ZnO can be naturally transferred into the black phosphorus by the energy band structure, and the excessive electrons in the black phosphorus can slow down the oxidation of the black phosphorus, thereby achieving the effect of passivating the surface of the black phosphorus. The method for passivating the black phosphorus nano material provided by the invention is simple and easy to implement and low in cost, and the prepared ZnO nanocrystal and black phosphorus nano material composite structure can greatly improve the stability of the black phosphorus nano material.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (7)
1. A method for passivating black phosphorus nano-materials is characterized by comprising the following steps:
A. grinding the black phosphorus blocks, dispersing the ground black phosphorus blocks into an N-methyl pyrrolidone solution, and performing ultrasonic treatment for 5-8 hours to obtain black phosphorus mixed solutions with different sizes;
B. carrying out step-by-step centrifugal treatment on the black phosphorus mixed solution by using a centrifugal force with a preset gradient to obtain a black phosphorus quantum dot colloidal solution;
C. adding Zn (CH) into the black phosphorus quantum dot colloidal solution under the inert gas atmosphere3COO)2Refluxing in water bath at 50-70 deg.C for 60-120min to obtain acetate precursor solution;
D. adding a pre-prepared N-methylpyrrolidone saturated solution of KOH into the acetate precursor solution, and reacting at the constant temperature of 50-60 ℃ for 120-210min to obtain a precipitate with a composite structure of ZnO nanocrystals and the black phosphorus nano material, thereby realizing the passivation of the black phosphorus nano material.
2. The method of passivating black phosphorus nanomaterials of claim 1, wherein the Zn (CH)3COO)2The mol ratio of the black phosphorus quantum dots to the black phosphorus quantum dots is 1:0.1-1: 0.5.
3. The method for passivating black phosphorus nanomaterials of claim 1, wherein the saturated solution of KOH in N-methylpyrrolidone is prepared by:
dissolving KOH in N-methylpyrrolidone solution, stirring for 30-60min at 50-70 ℃, and filtering to obtain the N-methylpyrrolidone saturated solution of KOH.
4. A method of passivating black phosphorus nanomaterials as recited in claim 3, wherein the Zn (CH)3COO)2The molar ratio to KOH is from 1:1.67 to 1: 2.
5. A method of passivating black phosphorus nanomaterials as claimed in claim 1, wherein the predetermined gradient of centrifugal force is: 70 Xg-20000 Xg, wherein g =9.80m/s2。
6. A method of passivating black phosphorus nanomaterials as recited in claim 1, wherein the inert gas is one or more of nitrogen, argon, helium, or neon.
7. The method of passivating black phosphorus nanomaterials of claim 1, further comprising, after step D:
E. and (3) cooling with cold water to terminate the reaction, and then centrifugally washing with N-methyl pyrrolidone for 3 times to obtain the purified ZnO nanocrystal and black phosphorus nanomaterial composite structure precipitate.
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