CN111137866A - Method for preparing boron nitride nanosheet by efficiently stripping h-BN - Google Patents
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Abstract
The invention discloses a method for preparing Boron Nitride Nanosheets (BNNS) by efficiently stripping hexagonal boron nitride (h-BN), which comprises the following steps: adding the h-BN powder and the surfactant into a first solvent, and uniformly stirring to obtain a first dispersion liquid; then carrying out ultrasonic treatment to obtain a second dispersion liquid; carrying out hydrothermal reaction on the second dispersion liquid to obtain a third dispersion liquid; then carrying out ultrasonic treatment to obtain a fourth dispersion liquid; centrifuging the fourth dispersion; centrifuging the obtained supernatant to obtain a precipitate, pouring a second solvent into the precipitate, uniformly stirring, and performing ultrasonic treatment to obtain a fifth dispersion; and (4) repeatedly centrifuging the fifth dispersion liquid, removing impurities from the obtained precipitate, and drying in vacuum to obtain BNNS. The method uses sodium citrate as a surfactant and provides ions for intercalation, combines liquid-phase ultrasonic dispersion and high-temperature high-pressure reaction to strip h-BN efficiently to prepare BNNS.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to a method for preparing Boron Nitride Nanosheets (BNNS) by efficiently stripping hexagonal boron nitride (h-BN).
Background
Boron Nitride (BN) is a ceramic material, and has good chemical stability, oxidation resistance, high thermal conductivity, electrical insulation and wide application prospect. Boron nitride is a crystal composed of nitrogen atoms and boron atoms, and has various crystal forms such as hexagonal, cubic, amorphous and the like, wherein hexagonal boron nitride (h-BN) is the most common crystal form and has a layered structure similar to a graphite structure, so that the boron nitride is also called as white graphite.
Boron Nitride Nanosheets (BNNS) are two-dimensional nanomaterials with a single-layer lattice structure similar to graphene, and have ultrahigh thermal conductivity (about 2000 W.m)-1K-1) Wide energy gap (about 5.9eV), high thermal stability and high length-diameter ratio, compared with bulk h-BN, the BNNS has more excellent performance, so that the BNNS becomes a new generation of ideal filler for preparing high-thermal-conductivity insulating dielectric materials.
The existing BNNS material preparation method mainly comprises a bottom-up synthesis method and a top-down stripping method, wherein the synthesis method mainly comprises a chemical vapor deposition method, and the method has high preparation cost and low yield and is difficult to realize large-scale production. The stripping method mainly includes a mechanical stripping method and a chemical stripping method. The mechanical stripping method mainly comprises a tape stripping method, a ball milling method, a fluid stripping method, a plasma etching method and the like; the chemical stripping method mainly comprises a liquid phase ultrasonic method and a chemical functionalization method. The liquid phase ultrasonic stripping method is the most potential method for large-scale production of BNNS, and utilizes the interaction between solvent molecules and the surface of h-BN and assists long-time ultrasonic stripping to obtain BNNS. However, due to the strong van de Waals forces and localized ionic bond-like forces (lip-lip) between BN atomic layers, combined with very small interlayer distances (only
The BNNS is very easy to agglomerate and is not easy to peel from the h-BN, and the over-high ultrasonic power or the over-long ultrasonic time can cause certain damage to the structure of the BNNS, so that the BNNS with large and thin sheets can not be obtained, the excellent heat-conducting property can not be maintained, and the actual yield of the BNNS is very low. Therefore, the development of the h-BN stripping method with simple and efficient operation to obtain the BNNS with few layers and complete structure is the first difficulty for promoting the practical application of the BNNS.
Disclosure of Invention
In order to solve the technical problems, the invention discloses a method for preparing BNNS by efficiently stripping h-BN, which combines liquid-phase ultrasonic dispersion and high-temperature high-pressure reaction to efficiently strip h-BN powder to prepare BNNS.
The invention is realized by the following technical scheme:
a method for preparing BNNS by efficiently stripping h-BN comprises the following steps:
(1) preparing a first dispersion: adding the h-BN powder and the surfactant into a first solvent, and uniformly stirring to obtain a first dispersion liquid;
(2) carrying out ultrasonic treatment on the first dispersion liquid to obtain a second dispersion liquid;
(3) carrying out hydrothermal reaction on the second dispersion liquid to obtain a third dispersion liquid;
(4) and stirring the third dispersion liquid and then carrying out ultrasonic treatment to obtain a fourth dispersion liquid.
(5) Centrifuging the fourth dispersion to obtain supernatant and precipitate.
(6) And (5) centrifuging the supernatant obtained in the step (5) to obtain a precipitate, pouring a second solvent into the precipitate, uniformly stirring, and performing ultrasonic treatment to obtain a fifth dispersion.
(7) And (5) repeatedly carrying out the treatment of the step (6) on the fifth dispersion liquid, removing impurities from the obtained precipitate, and carrying out vacuum drying to obtain BNNS.
In the step (1), the first solvent is a combination of deionized water and an organic solvent, the volume ratio of the water to the organic solvent is 1: 1-5, preferably 1: 2-3, and the organic solvent is a mixed solution of one or more of isopropanol, N-Dimethylformamide (DMF), and N-methylpyrrolidone (NMP), preferably isopropanol.
Further, in the step (1), the surfactant is sodium citrate dihydrate crystal (Na)3C6H5O7·2H2O), the mass ratio of the h-BN powder to the sodium citrate crystals is 1: 1-10, preferably 1: 1-5, the volume ratio of the mass of the h-BN powder to the first solvent is 1: 2-10 mg/ml, preferably 1: 2-5 mg/ml, and the particle size of the h-BN powder is 1-30 mu m.
Further, in the step (2), ultrasonic treatment is carried out in an ultrasonic cleaning machine, and the power of ultrasonic is 200 +/-2W; the ultrasonic frequency is 40 +/-2 kHz; the ultrasonic treatment time is 100-140 min, preferably 120 min.
Further, in the step (3), the hydrothermal reaction is carried out in a hydrothermal reaction kettle, wherein the temperature in the hydrothermal reaction kettle is 160-220 ℃, and preferably 180-200 ℃; the reaction time is 24 +/-1 h.
Further, in the step (4), ultrasonic treatment is carried out in an ultrasonic cleaning machine, and the ultrasonic power is 100 +/-2W; the ultrasonic frequency is 40 kHz; the ultrasonic treatment time is 3-5 min.
Further, in the step (5), the rotating speed of a centrifugal machine adopted for centrifugation is 1000 +/-100 rpm; the centrifugation time is 5-10 min.
Further, in the step (6), the rotating speed of a centrifugal machine used for centrifugation is 10000 +/-1000 rpm; the centrifugation time is 5-10 min, and the second solvent is isopropanol.
Further, in the step (6), ultrasonic treatment is carried out in an ultrasonic cleaning machine, the power of ultrasonic is 100 +/-2W, and the ultrasonic frequency is 40 +/-2 kHz; the ultrasonic treatment time is 3-5 min.
Further, in the step (7), the repeated treatment times of the step (6) are 3-5 times, the vacuum drying temperature is 40 +/-1 ℃, and the drying time is 48 +/-1 h.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention relates to an efficient peeling machineMethod for preparing BNNS by separating h-BN, sodium citrate dihydrate crystal (Na)3C6H5O7·2H2O) is dissolved in the organic mixed solution, and sodium ions Na are dispersed by ultrasonic+The method comprises the following steps of performing interlayer insertion on BNNS, allowing an anionic surfactant citrate to act on the surface of the BNNS to improve the surface energy of the BNNS, separating the BNNS in a hydrothermal reaction kettle by using thermal expansion, and realizing efficient stripping of h-BN by combining ultrasonic dispersion and high-temperature high-pressure reaction to obtain the BNNS with complete structure, few defects, thin thickness and good dispersibility;
2. the invention relates to a method for preparing BNNS (BNNS) by efficiently stripping h-BN (boron nitride). sodium ions (Na) dissolved in sodium citrate are dispersed in h-BN by a liquid-phase ultrasonic method+) Completely dispersing the dispersion into a dispersion liquid, intercalating the dispersion in a BNNS, and then putting the whole dispersion system in a high-temperature and high-pressure environment for hydrothermal reaction, wherein the strong van de Waals acting force between layers can be overcome due to the action of thermal expansion between BNNS layers, so that further stripping is realized;
3. the method for preparing BNNS by efficiently stripping h-BN has the advantages of low cost, simple and easily-controlled operation, high yield and good quality of the prepared BNNS, and is suitable for industrial production.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
FIG. 1 is a schematic representation of the stripping of h-BN to BNNS.
FIG. 2 is a dispersion solution of h-BN in isopropanol (after one week of standing).
FIG. 3 is a dispersion solution of BNNS prepared in example 1 in isopropanol (after standing for one week).
FIG. 4 is a Transmission Electron Microscope (TEM) photograph of unstripped h-BN.
FIG. 5 is a Scanning Electron Microscope (SEM) photograph of non-exfoliated h-BN.
FIG. 6 is a Transmission Electron Microscope (TEM) photograph of BNNS obtained in example 1.
FIG. 7 is a Scanning Electron Microscope (SEM) photograph of the BNNS prepared in example 1.
FIG. 8 is a Transmission Electron Microscope (TEM) photograph of BNNS obtained in example 2.
FIG. 9 is a Scanning Electron Microscope (SEM) photograph of the BNNS prepared in example 2.
FIG. 10 is a Transmission Electron Microscope (TEM) photograph of BNNS obtained in example 3.
FIG. 11 is a Scanning Electron Microscope (SEM) photograph of the BNNS prepared in example 3.
FIG. 12 is a Transmission Electron Microscope (TEM) photograph of BNNS obtained in example 4.
FIG. 13 is a Scanning Electron Microscope (SEM) photograph of the BNNS obtained in example 4.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
Example 1
The invention relates to a method for preparing boron nitride nanosheets by efficiently stripping h-BN, which comprises the following specific steps:
(1) 150mg of sodium citrate dihydrate crystals were weighed into a beaker, and 15ml of deionized water was poured to dissolve the crystals with stirring, followed by addition of 25ml of isopropanol.
(2) Weighing h-BN 150mg, adding the h-BN into the beaker in the step (1), stirring and dispersing, putting the beaker into an ultrasonic cleaning machine for ultrasonic treatment for 2 hours, and setting the power to be 200W.
(3) Adding the solution obtained by the ultrasonic treatment in the step (2) into a hydrothermal reaction kettle (the volume is 100ml), and reacting for 24 hours at the temperature of 180 ℃.
(4) And (4) after uniformly stirring the solution obtained by the reaction in the step (3), putting the solution into an ultrasonic cleaning machine for ultrasonic treatment for 3min, and setting the power to be 100W.
(5) And (4) carrying out low-speed centrifugation treatment on the solution obtained in the step (4), wherein the rotation speed of a centrifugal machine is 1000rpm, the time is 5min, after the centrifugation is finished, taking the supernatant as a BNNS dispersion liquid, and obtaining the precipitate which is not peeled h-BN after the centrifugation.
(6) And (4) carrying out high-speed centrifugation treatment on the supernatant obtained in the step (6), wherein the rotation speed of a centrifugal machine is 10000rpm, the time is 5min, collecting the sediment BNNS after the centrifugation is finished, pouring a small amount of isopropanol into the collected BNNS, and putting the BNNS into an ultrasonic cleaning machine for ultrasonic treatment for 3min, wherein the power is set to 100W.
(7) And (4) performing high-speed centrifugation treatment on the solution obtained in the step (6), repeating the step (6) for 3 times, repeatedly cleaning to remove residual impurities such as sodium citrate and the like, and collecting the finally obtained precipitate, putting the precipitate into a vacuum oven, and drying for 48 hours at 40 ℃ to obtain BNNS.
The TEM image and the SEM image of the BNNS prepared in this example are shown in FIG. 6 and FIG. 7, respectively. As can be seen from the electron microscope pictures, the BNNS sheet obtained in example 1 is very thin, and most of the sheet has larger transverse dimension and the diameter is about 5 μm. And the BNNS obtained by centrifugation in the example has 82.2mg and the yield reaches 54.8 percent, which shows that the stripping effect of the example 1 on the h-BN is very good.
Example 2
The invention relates to a method for preparing boron nitride nanosheets by efficiently stripping h-BN, which comprises the following specific steps:
(1) 150mg of sodium citrate was weighed into a beaker, 10ml of deionized water was poured to dissolve it with stirring, and then 25ml of DMF was added.
(2) Weighing h-BN 150mg, adding the h-BN into the beaker in the step (1), stirring and dispersing, putting the beaker into an ultrasonic cleaning machine for ultrasonic treatment for 2 hours, and setting the power to be 200W.
(3) Adding the solution obtained by the ultrasonic treatment in the step (2) into a hydrothermal reaction kettle (the volume is 100ml), and reacting for 24 hours at the temperature of 180 ℃.
(4) And (4) after uniformly stirring the solution obtained by the reaction in the step (3), putting the solution into an ultrasonic cleaning machine for ultrasonic treatment for 3min, and setting the power to be 100W.
(5) And (4) carrying out low-speed centrifugation treatment on the solution obtained in the step (4), wherein the rotation speed of a centrifugal machine is 1000rpm, the time is 5min, after the centrifugation is finished, taking the supernatant as a BNNS dispersion liquid, and obtaining the precipitate which is not peeled h-BN after the centrifugation.
(6) And (4) carrying out high-speed centrifugation treatment on the supernatant obtained in the step (6), wherein the rotation speed of a centrifugal machine is 10000rpm, the time is 5min, collecting the sediment BNNS after the centrifugation is finished, pouring a small amount of isopropanol into the collected BNNS, and putting the BNNS into an ultrasonic cleaning machine for ultrasonic treatment for 3min, wherein the power is set to 100W.
(7) And (4) performing high-speed centrifugation treatment on the solution obtained in the step (6), repeating the step (6) for 3 times, repeatedly cleaning to remove residual impurities such as sodium citrate and the like, and collecting the finally obtained precipitate, putting the precipitate into a vacuum oven, and drying for 48 hours at 40 ℃ to obtain BNNS.
The TEM image and the SEM image of the BNNS prepared in this example are shown in FIG. 8 and FIG. 9, respectively. It can be seen that the thickness of BNNS is relatively thick compared to example 1, which gives a BNNS yield of 45.6% upon centrifugation, indicating that aqueous DMF stripped h-BN less efficiently than aqueous isopropanol.
Example 3
This example differs from example 1 only in that: no sodium citrate was added.
The TEM image and the SEM image of the BNNS prepared in this example are shown in FIG. 10 and FIG. 11, respectively. It can be seen that the stripping effect of h-BN is deteriorated compared to examples 1 and 2, which gave a BNNS yield of 20.8% by centrifugation, indicating that sodium citrate had a significant effect on the stripping effect of h-BN.
Example 4
This example differs from example 1 only in that: and (3) omitting the step (3), and directly carrying out ultrasonic treatment in the step (4) after the step (2) is finished.
The TEM image and the SEM image of the BNNS prepared in this example are shown in FIG. 12 and FIG. 13, respectively. It can be seen that the BNNS is thicker compared to example 1, which gives a BNNS yield of 17.5% upon centrifugation, indicating that high temperature and pressure have a significant effect on the exfoliation effect of h-BN.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A method for preparing BNNS by efficiently stripping h-BN is characterized by comprising the following steps:
(1) preparing a first dispersion: adding the h-BN powder and the surfactant into a first solvent, and uniformly stirring to obtain a first dispersion liquid;
(2) carrying out ultrasonic treatment on the first dispersion liquid to obtain a second dispersion liquid;
(3) carrying out hydrothermal reaction on the second dispersion liquid to obtain a third dispersion liquid;
(4) and stirring the third dispersion liquid and then carrying out ultrasonic treatment to obtain a fourth dispersion liquid.
(5) Centrifuging the fourth dispersion to obtain supernatant and precipitate.
(6) And (5) centrifuging the supernatant obtained in the step (5) to obtain a precipitate, pouring a second solvent into the precipitate, uniformly stirring, and performing ultrasonic treatment to obtain a fifth dispersion.
(7) And (5) repeatedly carrying out the treatment of the step (6) on the fifth dispersion liquid, removing impurities from the obtained precipitate, and carrying out vacuum drying to obtain BNNS.
2. The method for preparing BNNS by efficiently stripping h-BN according to claim 1, wherein in the step (1), the first solvent is a combination of deionized water and an organic solvent, the volume ratio of the water to the organic solvent is 1: 1-5, and the organic solvent is one or more of isopropanol, N-dimethylformamide and N-methylpyrrolidone.
3. The method for preparing BNNS by efficiently peeling off h-BN according to claim 1, wherein in the step (1), the surfactant is sodium citrate dihydrate crystals, the mass ratio of the h-BN to the sodium citrate crystals is 1: 1-10, the volume ratio of the mass of the BN powder to the first solvent is 1: 2-10 mg/ml, and the particle size of the h-BN powder is 1-30 μm.
4. The method for preparing BNNS by efficiently peeling h-BN according to claim 1, wherein in the step (2), the ultrasonic treatment is performed in an ultrasonic cleaning machine, and the power of the ultrasonic is 200 +/-2W; the ultrasonic frequency is 40 +/-2 kHz; the ultrasonic treatment time is 100-140 min.
5. The method for preparing BNNS by efficiently stripping h-BN according to claim 1, wherein in the step (3), the hydrothermal reaction is carried out in a hydrothermal reaction kettle, the temperature in the hydrothermal reaction kettle is 160-220 ℃, and the reaction time is 24 +/-1 h.
6. The method for preparing BNNS by efficiently peeling h-BN according to claim 1, wherein in the step (4), the ultrasonic treatment is performed in an ultrasonic cleaning machine, and the ultrasonic power is 100 +/-2W; the ultrasonic frequency is 40 kHz; the ultrasonic treatment time is 3-5 min.
7. The method for preparing BNNS by efficiently stripping h-BN according to claim 1, wherein in the step (5), the rotation speed of a centrifuge used for centrifugation is 1000 +/-100 rpm; the centrifugation time is 5-10 min.
8. The method for preparing BNNS by efficiently stripping h-BN according to claim 1, wherein in the step (6), the rotation speed of a centrifuge used for centrifugation is 10000 +/-1000 rpm; the centrifugation time is 5-10 min, and the second solvent is isopropanol.
9. The method for preparing BNNS by efficiently stripping h-BN according to claim 1, wherein in the step (6), the ultrasonic treatment is performed in an ultrasonic cleaning machine, the power of the ultrasonic is 100 +/-2W, and the ultrasonic frequency is 40 +/-2 kHz; the ultrasonic treatment time is 3-5 min.
10. The method for preparing BNNS by efficiently stripping h-BN according to claim 1, wherein in the step (7), the number of times of the repeated treatment of the step (6) is 3-5, the temperature of the vacuum drying is 40 +/-1 ℃, and the drying time is 48 +/-1 h.
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| CN111717900A (en) * | 2020-07-06 | 2020-09-29 | 河北工业大学 | Mechanical stripping method of functionalized boron nitride nanosheets |
| CN114479774A (en) * | 2022-01-20 | 2022-05-13 | 国网河北省电力有限公司电力科学研究院 | Preparation method and preparation equipment of heat-conducting insulating material GBN |
| CN116457303A (en) * | 2020-09-21 | 2023-07-18 | 迪金大学 | Production of boron nitride nanoplatelets |
| WO2023149999A1 (en) * | 2022-02-04 | 2023-08-10 | The Penn State Research Foundation | Methods for preparing alkali metal-intercalated hexagonal boron nitride materials, resultant products and uses thereof |
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| CN114479774A (en) * | 2022-01-20 | 2022-05-13 | 国网河北省电力有限公司电力科学研究院 | Preparation method and preparation equipment of heat-conducting insulating material GBN |
| CN114479774B (en) * | 2022-01-20 | 2023-09-26 | 国网河北省电力有限公司电力科学研究院 | Preparation method and preparation equipment of heat-conducting insulating material GBN |
| WO2023149999A1 (en) * | 2022-02-04 | 2023-08-10 | The Penn State Research Foundation | Methods for preparing alkali metal-intercalated hexagonal boron nitride materials, resultant products and uses thereof |
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