CN111807335A - Microwave-assisted method for preparing boron nitride nanosheets - Google Patents
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Abstract
The invention discloses a microwave-assisted method for preparing boron nitride nanosheets, which comprises the steps of dispersing h-BN powder in deionized water, and fully dispersing the h-BN powder by means of ultrasound to form a water phase system; transferring the dispersed h-BN dispersion liquid into a microwave digestion instrument for digestion at a certain temperature, time and pressure; further carrying out ultrasonic treatment on the digested dispersion liquid at certain power and time to further strip the h-BN; centrifuging the ultrasonic dispersion liquid at different rotating speeds and time to finally obtain centrifuged lower-layer precipitate; and finally, carrying out vacuum drying on the obtained lower-layer precipitate at a certain temperature and for a certain time to obtain single-layer or few-layer BNNS. Through detection, the manufactured BNNS has a thinner thickness and a transverse dimension of 100-200 nm.
Description
Technical Field
The invention relates to a microwave-assisted method for preparing boron nitride nanosheets, and belongs to the field of preparation of heat conducting materials.
Background
Boron Nitride Nanosheets (BNNS) are excellent two-dimensional materials with a graphene-like layered structure and are therefore also referred to as white graphite. The boron nitride nanosheets are mainly different from graphene in that the boron nitride nanosheets have high insulating property, high thermal conductivity (1700-2000W/m K), excellent mechanical properties and the like, and are ideal heat conducting materials. BNNS can be prepared from hexagonal boron nitride (h-BN) powder, has larger specific surface area and better dispersibility compared with three-dimensional h-BN, can form more perfect heat conduction paths in materials, and can be used as heat conduction filler with excellent performance to prepare polymer composite materials with high heat conductivity and insulativity. It was found that due to the small h-BN layer spacing, ionic bonding exists between layers, making BNNS difficult to exfoliate into a single sheet from a three-dimensional h-BN mass.
Common methods for stripping BNNS mainly comprise a mechanical grinding method, a molten hydroxide etching method, an electrochemical stripping method, a liquid phase stripping method and the like. However, these methods generally require harsh chemical conditions and are not environmentally friendly, and the challenge of preparing BNNS with uniform size and high yield is still facing. The hydrothermal method is a method capable of generating higher pressure at low temperature so as to promote the formation of the metastable nano structure, can effectively reduce the stripping energy of h-BN, and is a method for preparing BNNS with strong operability, economy and environmental protection. In addition, microwave heating means that electromagnetic waves with the frequency of 300 MHz-300 GHz are utilized, the heated materials are subjected to microwave radiation, and internal particles move in an accelerated mode to generate collision and friction, so that a thermal effect is generated. Compared with the traditional heating mode, the microwave heating has the characteristics of high heating speed, uniform heating, easiness in control, energy conservation, high efficiency and the like, and can save a large amount of time and energy.
A micro-assisted hydrothermal method is designed by utilizing the characteristics of microwave heating and the hydrothermal reaction principle and is used for stripping preparation of BNNS. The method has the characteristics of energy conservation, high efficiency, cleanness, no pollution and the like, and has important significance for large-scale preparation of high-quality BNNS.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a microwave-assisted method for preparing boron nitride nanosheets, which utilizes the characteristics of rapidness, uniformity, energy conservation, high efficiency and the like of microwave heating and combines a high-pressure environment provided by hydrothermal reaction, so that the interlayer acting force of h-BN is effectively overcome, and the h-BN is stripped and fallen into single-layer or few-layer BNNS.
In order to achieve the purpose, the invention adopts the following technical means:
a method for preparing boron nitride nanosheets with the assistance of microwaves comprises the following steps:
(1) dispersing the h-BN powder in deionized water, and carrying out ultrasonic treatment to obtain h-BN dispersion liquid;
(2) digesting the h-BN dispersion liquid at the digestion temperature of 100-300 ℃ for 2-4 h, keeping the temperature for 10-40 min and keeping the pressure at 30-50 atm;
(3) carrying out ultrasonic stripping treatment on the digested dispersion liquid, wherein the ultrasonic power is 300-600W, and the ultrasonic time is 10-20 min;
(4) centrifuging the mixed system after ultrasonic treatment;
(5) and drying the centrifuged lower-layer substance to obtain the boron nitride nanosheet.
As a further improvement of the invention, in the step (1), the proportion of the h-BN dispersion liquid is that every 100-300 mg of h-BN powder is dispersed in 30-100 ml of deionized water.
As a further improvement of the invention, in the step (2), the h-BN dispersion is placed in a microwave digestion instrument for digestion.
As a further improvement of the invention, in the step (4), the centrifugation time is 5-15 min, and the rotating speed is 2000-9000 rpm.
As a further improvement of the invention, in the step (5), the centrifuged lower-layer substance is dried in vacuum at the drying temperature of 70-110 ℃ for 10-30 h.
As a further improvement of the invention, the boron nitride nanosheet is flaky, and the transverse dimension of the boron nitride nanosheet is 100-200 nm.
Compared with the prior art, the invention has the following advantages:
according to the method, deionized water is used as a solvent, microwave-assisted hydrothermal reaction is utilized, the stripping energy of h-BN can be effectively reduced, the dispersion liquid after ultrasonic treatment is subjected to centrifugal treatment at different rotating speeds and time, a product with a stable structure is obtained, BNNS with a large size (the transverse size is 100-200 nm) and a thin lamella is finally prepared, the whole preparation process is environment-friendly, the operation is simple, and the product quality is high. The prepared BNNS can be used as a heat-conducting insulating filler to prepare a heat-conducting insulating composite material with excellent performance. The method utilizes the characteristics of rapid and uniform microwave heating, energy conservation, high efficiency and the like, combines a high-pressure environment provided by hydrothermal reaction, effectively overcomes the interlayer acting force of h-BN, and promotes the h-BN to be stripped and fall into single-layer or few-layer BNNS. Meanwhile, the solvent used in the invention is deionized water, the whole preparation process is energy-saving and efficient, clean and pollution-free, and strong in operability, and the prepared BNNS has fewer layers and large size and is expected to be applied to large-scale production of BNNS.
Further, the centrifugal rotating speed of the multiple times of centrifugal treatment is sequentially increased, so that products which are not completely stripped can be further stripped.
Drawings
FIG. 1 is an SEM photograph of BNNS produced in example 1;
FIG. 2 is a TEM image of BNNS produced in example 1;
FIG. 3 is a Raman spectrum of BNNS prepared in example 1.
Detailed Description
The invention relates to a microwave-assisted method for preparing boron nitride nanosheets, which specifically comprises the following steps:
(1) dispersing 100-300 mg of h-BN powder in 30-100 ml of deionized water, and carrying out ultrasonic treatment for 10-30 min; the main purpose is: dispersing the h-BN powder in deionized water, and fully dispersing the h-BN powder by means of ultrasonic to form a water phase system;
(2) placing the dispersed h-BN dispersion liquid into a microwave digestion instrument for digestion, setting the digestion temperature to be 100-300 ℃, and the digestion time to be 2-4 h, wherein the main purposes are as follows: transferring the dispersed h-BN dispersion liquid into a microwave digestion instrument for digestion at a certain temperature, time and pressure;
(3) carrying out ultrasonic treatment on the digested dispersion liquid, wherein the ultrasonic power is 300-600W, and the ultrasonic time is 10-20 min; carrying out ultrasonic treatment on the digested dispersion liquid at certain power and time to further strip the h-BN;
(4) centrifuging the ultrasonic mixed system for 5-15 min at the rotating speed of 7000-9000 rpm; centrifuging the ultrasonic dispersion liquid at different rotating speeds and time to finally obtain centrifuged lower-layer sediment;
(5) and (4) drying the centrifuged lower-layer substance in vacuum at the drying temperature of 70-110 ℃ for 10-30 h. And drying the obtained lower-layer precipitate in vacuum at a certain temperature and for a certain time to obtain single-layer or few-layer BNNS.
The technical solutions of the present invention will be described in detail below with reference to specific examples and drawings, but the present invention is not limited to the examples.
Example 1
Preparing boron nitride nanosheets with microwave assistance: firstly, dispersing 150mg of h-BN powder in 30ml of deionized water, and carrying out ultrasonic dispersion for 10 min; transferring the dispersed h-BN dispersion liquid into a microwave digestion instrument, setting the microwave digestion temperature to be 180 ℃, the digestion time to be 2h, the heat preservation time to be 30min and the pressure to be 30 atm; further, carrying out ultrasonic treatment on the digested dispersion liquid, wherein the ultrasonic power is set to be 600W, and the ultrasonic time is 20 min; centrifuging the ultrasonic mixed system, setting the centrifugal speed to 3000rpm, centrifuging for 10min, removing the un-peeled h-BN precipitate on the lower layer, further continuously centrifuging the dispersion liquid on the upper layer, setting the centrifugal speed to 8000rpm, and centrifuging for 5min to obtain the precipitate on the lower layer; and finally, carrying out vacuum drying on the obtained lower-layer precipitate, setting the drying temperature to be 105 ℃, and drying for 24 hours to prepare the single-layer or few-layer BNNS.
The experimental results of this example were subjected to the relevant experimental tests, and the test results are shown in fig. 1 to 3.
In which, FIGS. 1 and 2 are SEM and TEM images of BNNS prepared in example 1 of the present invention, respectively, it can be seen that BNNS is in the form of sheet, has smooth edges and thin thickness, has a transverse dimension of about 100-200 nm, and has a small size of partial sheet due to the fragmentation of part of boron nitride during the ultrasonic process.
FIG. 3 is a Raman spectrum of BNNS prepared in example 1 of the present invention, from which it can be seen that the characteristic peak of original h-BN appears at 1365, while the characteristic peak corresponding to BNNS is red-shifted and the intensity of the G peak becomes lower due to the decrease in the number of sheets during the exfoliation of h-BN; furthermore, the half-peak width of BNNS is slightly larger than h-BN, also because the number of lamellae is reduced, the interlayer spacing is increased, and the surface scattering of BNNS is stronger than that of original BN. Therefore, the microwave-assisted preparation of the boron nitride nanosheet can prepare the BNNS with fewer layers and thinner lamella.
Example 2
Preparing boron nitride nanosheets with microwave assistance: firstly, dispersing 200mg of h-BN powder in 30ml of deionized water, and carrying out ultrasonic dispersion for 10 min; transferring the dispersed h-BN dispersion liquid into a microwave digestion instrument, setting the microwave digestion temperature to be 180 ℃, the digestion time to be 2h, the heat preservation time to be 30min and the pressure to be 30 atm; further, carrying out ultrasonic treatment on the digested dispersion liquid, wherein the ultrasonic power is set to be 600W, and the ultrasonic time is 20 min; centrifuging the ultrasonic mixed system, setting the centrifugal speed to 3000rpm, centrifuging for 10min, removing the un-peeled h-BN precipitate on the lower layer, further continuously centrifuging the dispersion liquid on the upper layer, setting the centrifugal speed to 8000rpm, and centrifuging for 5min to obtain the precipitate on the lower layer; and finally, carrying out vacuum drying on the obtained lower-layer precipitate, setting the drying temperature to be 105 ℃, and drying for 24 hours to prepare the single-layer or few-layer BNNS.
Example 3
Preparing boron nitride nanosheets with microwave assistance: firstly, dispersing 200mg of h-BN powder in 30ml of deionized water, and carrying out ultrasonic dispersion for 10 min; transferring the dispersed h-BN dispersion liquid into a microwave digestion instrument, setting the microwave digestion temperature to be 180 ℃, the digestion time to be 3h, the heat preservation time to be 30min and the pressure to be 30 atm; further, carrying out ultrasonic treatment on the digested dispersion liquid, wherein the ultrasonic power is set to be 600W, and the ultrasonic time is 20 min; centrifuging the ultrasonic mixed system, setting the centrifugal speed to 3000rpm, centrifuging for 10min, removing the un-peeled h-BN precipitate on the lower layer, further continuously centrifuging the dispersion liquid on the upper layer, setting the centrifugal speed to 8000rpm, and centrifuging for 5min to obtain the precipitate on the lower layer; and finally, carrying out vacuum drying on the obtained lower-layer precipitate, setting the drying temperature to be 105 ℃, and drying for 24 hours to prepare the single-layer or few-layer BNNS.
Example 4
Preparing boron nitride nanosheets with microwave assistance: firstly, dispersing 150mg of h-BN powder in 30ml of deionized water, and carrying out ultrasonic dispersion for 10 min; transferring the dispersed h-BN dispersion liquid into a microwave digestion instrument, setting the microwave digestion temperature to be 180 ℃, the digestion time to be 3h, the heat preservation time to be 30min and the pressure to be 30 atm; further, carrying out ultrasonic treatment on the digested dispersion liquid, wherein the ultrasonic power is set to be 600W, and the ultrasonic time is 20 min; centrifuging the ultrasonic mixed system, setting the centrifugal speed to 3000rpm, centrifuging for 10min, removing the un-peeled h-BN precipitate on the lower layer, further continuously centrifuging the dispersion liquid on the upper layer, setting the centrifugal speed to 8000rpm, and centrifuging for 5min to obtain the precipitate on the lower layer; and finally, carrying out vacuum drying on the obtained lower-layer precipitate, setting the drying temperature to be 105 ℃, and drying for 24 hours to prepare the single-layer or few-layer BNNS.
Example 5
Preparing boron nitride nanosheets with microwave assistance: firstly, dispersing 150mg of h-BN powder in 30ml of deionized water, and carrying out ultrasonic dispersion for 10 min; transferring the dispersed h-BN dispersion liquid into a microwave digestion instrument, setting the microwave digestion temperature to be 180 ℃, the digestion time to be 2h, the heat preservation time to be 30min and the pressure to be 30 atm; further, carrying out ultrasonic treatment on the digested dispersion liquid, wherein the ultrasonic power is set to be 400W, and the ultrasonic time is set to be 20 min; centrifuging the ultrasonic mixed system, setting the centrifugal speed to 3000rpm, centrifuging for 10min, removing the un-peeled h-BN precipitate on the lower layer, further continuously centrifuging the dispersion liquid on the upper layer, setting the centrifugal speed to 8000rpm, and centrifuging for 5min to obtain the precipitate on the lower layer; and finally, carrying out vacuum drying on the obtained lower-layer precipitate, setting the drying temperature at 105 ℃ and the drying time at 24h, and preparing the single-layer or few-layer BNNS.
Example 6
Preparing boron nitride nanosheets with microwave assistance: firstly, dispersing 150mg of h-BN powder in 30ml of deionized water, and carrying out ultrasonic dispersion for 10 min; transferring the dispersed h-BN dispersion liquid into a microwave digestion instrument, setting the microwave digestion temperature to be 180 ℃, the digestion time to be 4h, the heat preservation time to be 30min and the pressure to be 30 atm; further, carrying out ultrasonic treatment on the digested dispersion liquid, wherein the ultrasonic power is set to be 400W, and the ultrasonic time is set to be 20 min; centrifuging the ultrasonic mixed system, setting the centrifugal speed to 3000rpm, centrifuging for 10min, removing the un-peeled h-BN precipitate on the lower layer, further continuously centrifuging the dispersion liquid on the upper layer, setting the centrifugal speed to 8000rpm, and centrifuging for 5min to obtain the precipitate on the lower layer; and finally, carrying out vacuum drying on the obtained lower-layer precipitate, setting the drying temperature at 105 ℃ and the drying time at 24h, and preparing the single-layer or few-layer BNNS.
Example 7
Preparing boron nitride nanosheets with microwave assistance: firstly, dispersing 150mg of h-BN powder in 30ml of deionized water, and carrying out ultrasonic dispersion for 10 min; transferring the dispersed h-BN dispersion liquid into a microwave digestion instrument, setting the microwave digestion temperature to be 180 ℃, the digestion time to be 2h, the heat preservation time to be 30min and the pressure to be 30 atm; further, carrying out ultrasonic treatment on the digested dispersion liquid, wherein the ultrasonic power is set to be 600W, and the ultrasonic time is 10 min; centrifuging the ultrasonic mixed system, setting the centrifugal speed to 5000rpm, centrifuging for 10min, removing the un-peeled h-BN precipitate on the lower layer, further centrifuging the dispersion liquid on the upper layer, setting the centrifugal speed to 8000rpm, centrifuging for 5min, and obtaining the precipitate on the lower layer; and finally, carrying out vacuum drying on the obtained lower-layer precipitate, setting the drying temperature at 105 ℃ and the drying time at 24h, and preparing the single-layer or few-layer BNNS.
Example 8
Preparing boron nitride nanosheets with microwave assistance: firstly, dispersing 100mg of h-BN powder in 100ml of deionized water, and carrying out ultrasonic dispersion for 15 min; transferring the dispersed h-BN dispersion liquid into a microwave digestion instrument, setting the microwave digestion temperature to be 100 ℃, the digestion time to be 3h, the heat preservation time to be 10min and the pressure to be 40 atm; further, carrying out ultrasonic treatment on the digested dispersion liquid, wherein the ultrasonic power is set to be 300W, and the ultrasonic time is set to be 15 min; centrifuging the ultrasonic mixed system, setting the centrifugal speed at 2000rpm for 5min, removing the un-peeled h-BN precipitate on the lower layer, further continuously centrifuging the dispersion liquid on the upper layer, setting the centrifugal speed at 9000rpm for 15min, and obtaining the precipitate on the lower layer; and finally, carrying out vacuum drying on the obtained lower-layer precipitate, setting the drying temperature to be 75 ℃, and drying for 30h to prepare the single-layer or few-layer BNNS.
Example 9
Preparing boron nitride nanosheets with microwave assistance: firstly, dispersing 300mg of h-BN powder in 100ml of deionized water, and carrying out ultrasonic dispersion for 10 min; transferring the dispersed h-BN dispersion liquid into a microwave digestion instrument, setting the microwave digestion temperature to be 300 ℃, the digestion time to be 4h, the heat preservation time to be 40min and the pressure to be 50 atm; further, carrying out ultrasonic treatment on the digested dispersion liquid, wherein the ultrasonic power is set to be 400W, and the ultrasonic time is set to be 20 min; centrifuging the ultrasonic mixed system, setting the centrifugal speed to 3000rpm, centrifuging for 6min, removing the un-peeled h-BN precipitate on the lower layer, further centrifuging the dispersion liquid on the upper layer, setting the centrifugal speed to 7000rpm, and centrifuging for 10min to obtain the precipitate on the lower layer; and finally, carrying out vacuum drying on the obtained lower-layer precipitate, setting the drying temperature at 110 ℃, and drying for 30h to prepare the single-layer or few-layer BNNS.
Therefore, the invention discloses a microwave-assisted method for preparing boron nitride nanosheets, which comprises the steps of dispersing h-BN powder in deionized water, and fully dispersing the h-BN powder by means of ultrasound to form a water phase system; transferring the dispersed h-BN dispersion liquid into a microwave digestion instrument for digestion at a certain temperature, time and pressure; further carrying out ultrasonic treatment on the digested dispersion liquid at certain power and time to further strip the h-BN; centrifuging the ultrasonic dispersion liquid at different rotating speeds and time to finally obtain centrifuged lower-layer precipitate; and finally, carrying out vacuum drying on the obtained lower-layer precipitate at a certain temperature and for a certain time to obtain single-layer or few-layer BNNS. Through detection, the manufactured BNNS has a thinner thickness and a transverse dimension of 100-200 nm. The method has the advantages of environmental protection, simple operation, high product quality and the like, and the method utilizes the characteristics of rapid and uniform microwave heating, energy conservation, high efficiency and the like, has the advantages of energy conservation, high efficiency, cleanness, no pollution and strong operability in the whole preparation process, and is expected to be applied to the large-scale production of BNNS.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (7)
1. A method for preparing boron nitride nanosheets with the assistance of microwaves is characterized by comprising the following steps:
(1) dispersing the h-BN powder in deionized water, and carrying out ultrasonic treatment to obtain h-BN dispersion liquid;
(2) digesting the h-BN dispersion liquid at the digestion temperature of 100-300 ℃ for 2-4 h, keeping the temperature for 10-40 min and keeping the pressure at 30-50 atm;
(3) carrying out ultrasonic stripping treatment on the digested dispersion liquid, wherein the ultrasonic power is 300-600W, and the ultrasonic time is 10-20 min;
(4) carrying out multiple times of centrifugal treatment on the mixed system after ultrasonic treatment at different rotating speeds and time;
(5) and drying the centrifuged lower-layer substance to obtain the boron nitride nanosheet.
2. The microwave-assisted method for preparing boron nitride nanosheets of claim 1, wherein: in the step (1), the h-BN dispersion liquid is dispersed in 30-100 ml of deionized water according to the proportion of 100-300 mg of h-BN powder.
3. The microwave-assisted method for preparing boron nitride nanosheets of claim 1, wherein: and (2) digesting the h-BN dispersion liquid in a microwave digestion instrument.
4. The microwave-assisted method for preparing boron nitride nanosheets of claim 1, wherein: in the step (4), the centrifugal rotating speeds of the multiple times of centrifugal treatment are sequentially increased.
5. The microwave-assisted method for preparing boron nitride nanosheets of claim 1, wherein: in the step (4), the centrifugation time is 5-15 min, and the rotating speed is 2000-9000 rpm.
6. The microwave-assisted method for preparing boron nitride nanosheets of claim 1, wherein: and (5) carrying out vacuum drying on the centrifuged lower-layer substance at the drying temperature of 70-110 ℃ for 10-30 h.
7. The microwave-assisted method for preparing boron nitride nanosheets of claim 1, wherein: the boron nitride nanosheet is flaky, and the transverse dimension of the boron nitride nanosheet is 100-200 nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113013425A (en) * | 2021-02-22 | 2021-06-22 | 南京航空航天大学 | Difunctional anion-doped MPS3Catalyst, preparation method and application thereof |
| CN113213437A (en) * | 2021-05-31 | 2021-08-06 | 陕西科技大学 | Boron nitride nanosheet and preparation method thereof |
| 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 |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20170023345A (en) * | 2015-08-21 | 2017-03-03 | 한국세라믹기술원 | Method for preparing dispersion sol of boron nitride nanosheet by microwave heating and dispersion sol of boron nitride nanosheet prepared by the method |
| CN107055491A (en) * | 2017-04-28 | 2017-08-18 | 武汉理工大学 | A kind of method that utilization urea assisting ultrasonic prepares hexagonal boron nitride nanosheet |
| CN108046250A (en) * | 2017-12-22 | 2018-05-18 | 江苏大学 | A kind of preparation method of two-dimensional material |
| CN109205578A (en) * | 2018-08-09 | 2019-01-15 | 上海交通大学 | A kind of method of microwave-assisted liquid phase stripped laminar material preparation two-dimensional nano piece |
| CN109573965A (en) * | 2018-12-26 | 2019-04-05 | 合肥学院 | A kind of preparation method of hydroxyl modification boron nitride nanosheet dispersion liquid |
| CN110562938A (en) * | 2019-10-15 | 2019-12-13 | 燕山大学 | Method for stripping hexagonal boron nitride by microwave |
| CN110668408A (en) * | 2019-11-08 | 2020-01-10 | 常熟理工学院 | Preparation method of high-yield large-size boron nitride nanosheet |
-
2020
- 2020-07-08 CN CN202010653673.2A patent/CN111807335B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20170023345A (en) * | 2015-08-21 | 2017-03-03 | 한국세라믹기술원 | Method for preparing dispersion sol of boron nitride nanosheet by microwave heating and dispersion sol of boron nitride nanosheet prepared by the method |
| CN107055491A (en) * | 2017-04-28 | 2017-08-18 | 武汉理工大学 | A kind of method that utilization urea assisting ultrasonic prepares hexagonal boron nitride nanosheet |
| CN108046250A (en) * | 2017-12-22 | 2018-05-18 | 江苏大学 | A kind of preparation method of two-dimensional material |
| CN109205578A (en) * | 2018-08-09 | 2019-01-15 | 上海交通大学 | A kind of method of microwave-assisted liquid phase stripped laminar material preparation two-dimensional nano piece |
| CN109573965A (en) * | 2018-12-26 | 2019-04-05 | 合肥学院 | A kind of preparation method of hydroxyl modification boron nitride nanosheet dispersion liquid |
| CN110562938A (en) * | 2019-10-15 | 2019-12-13 | 燕山大学 | Method for stripping hexagonal boron nitride by microwave |
| CN110668408A (en) * | 2019-11-08 | 2020-01-10 | 常熟理工学院 | Preparation method of high-yield large-size boron nitride nanosheet |
Non-Patent Citations (2)
| Title |
|---|
| 田兆波等: "微波水热剥离制备高结晶六方氮化硼纳米片", 《稀有金属材料与工程》, vol. 49, no. 2, 29 February 2020 (2020-02-29), pages 1 * |
| 鲍婕: "二维层状六方氮化硼在高功率电子器件中的绝缘散热应用研究", 《中国优秀博硕士学位论文全文数据库(博士) 信息科技辑》, no. 02, 15 February 2017 (2017-02-15), pages 2 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113013425A (en) * | 2021-02-22 | 2021-06-22 | 南京航空航天大学 | Difunctional anion-doped MPS3Catalyst, preparation method and application thereof |
| CN113013425B (en) * | 2021-02-22 | 2022-11-15 | 南京航空航天大学 | Difunctional anion-doped MPS 3 Catalyst, preparation method and application thereof |
| CN113213437A (en) * | 2021-05-31 | 2021-08-06 | 陕西科技大学 | Boron nitride nanosheet and preparation method thereof |
| 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 |
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