CN108529573A - A method of preparing hexagonal boron nitride nanosheet using molten caustic soda and ultrasonic lift-off technology - Google Patents
A method of preparing hexagonal boron nitride nanosheet using molten caustic soda and ultrasonic lift-off technology Download PDFInfo
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Abstract
The present invention relates to a kind of methods preparing hexagonal boron nitride nanosheet using molten caustic soda and ultrasonic lift-off technology.Specifically, the method combines ultrasonic lift-off technology that hexagonal boron nitride nanosheet is prepared using molten caustic soda preconditioning technique.The invention also discloses using hexagonal boron nitride nanosheet made from the method.The method has the characteristics that simple for process, at low cost, safety non-pollution, can rapidly and efficiently prepare hexagonal boron nitride nanosheet.
Description
Technical field
The present invention relates to Material Fields, and six sides nitridation is prepared using molten caustic soda and ultrasonic lift-off technology more particularly to a kind of
The method of boron nanometer sheet.
Background technology
Two-dimensional layer material (material thickness is between 1nm to 100nm) in nano material possesses special physical chemistry
Characteristic and it is numerous it is potential application and paid attention to by more and more people.Among these two-dimensional layer nano materials, six side's nitrogen
Change boron nanometer sheet (h-BNNs) because its in structure it is similar with graphene due to have received widespread attention, chemical stability, heat
The performances such as stability are particularly excellent, therefore have more outstanding performance compared with graphene in some fields h-BNNs, for example make
Standby highly thermally conductive ceramic component, heat conductive insulating composite material and recoverable adsorbent etc..
Up to the present, the method for preparing h-BNNs is not very much, mainly there is chemical vapor deposition method, mechanical stripping method
With liquid phase stripping method, wherein liquid phase stripping method yield in theory is higher.But between layers due to hexagonal boron nitride
With stronger ionic bond effect so that the yield that traditional liquid phase lift-off technology prepares h-BNNs is actually very low.
Therefore, there is an urgent need in the art to a kind of new technologies to remove hexagonal boron nitride nanosheet.
Invention content
The purpose of the present invention is to provide a kind of technologies of new stripping hexagonal boron nitride nanosheet.
The first aspect of the present invention provides a kind of method preparing hexagonal boron nitride nanosheet, and the method includes such as
Lower step：
1) the first mixed liquor is provided, first mixed liquor includes the first solvent and is scattered among first solvent
Through the pretreated hexagonal boron nitride powder of molten caustic soda；
2) it is ultrasonically treated first mixed liquor, obtains the second mixed liquor；
3) optionally the second mixed liquor described in filtration treatment, and precipitation obtained by carrying out washing treatment, and products therefrom is disperseed again
In the second solvent, third mixed liquor is obtained；
4) centrifugal treating abovementioned steps products therefrom, collects upper layer dispersion liquid, and drying process obtains hexagonal nanometer boron nitride
Piece.
In another preferred example, first solvent and second solvent are water, preferably deionized water.
In another preferred example, after step 4), following steps are also optionally included：
5) centrifugation gained sediment in step 4) is scattered in again in the second solvent, adds alkaline matter, it is mixed obtains the 4th
Close liquid；
6) step 2) -4 is repeated), difference is：First mixed liquor is replaced with the 4th mixed liquor.
In another preferred example, step 5) -6 is repeated), it is preferable that number of repetition is 1-5 times.
In another preferred example, described to be prepared as follows through the pretreated hexagonal boron nitride powder of molten caustic soda：
A-1) alkaline matter and hexagonal boron nitride powder are provided；
A-2 the alkaline matter and the hexagonal boron nitride powder) are mixed, the first mixture is obtained；
A-3) the first mixture described in high-temperature process obtains described through the pretreated hexagonal boron nitride powder of molten caustic soda.
In another preferred example, the grain size of the hexagonal boron nitride powder is 1-20 μm, preferably 3-18 μm, more preferably 4-
15μm。
In another preferred example, the alkaline matter is selected from the group：Sodium hydroxide, potassium hydroxide, or combinations thereof.
In another preferred example, the alkaline matter is the mixture of sodium hydroxide and potassium hydroxide.
In another preferred example, in the alkaline matter, the mass mixing ratio of sodium hydroxide and potassium hydroxide is 0.1-5,
Preferably 0.3-3, more preferably 0.5-2.5.
In another preferred example, in first mixture, the matter of the alkaline matter and the hexagonal boron nitride powder
Amount ratio is 1-20, preferably 1-10, more preferably 1-6.
In another preferred example, the treatment temperature of the high-temperature process be 100-300 DEG C, preferably 120-260 DEG C, more preferably
140-240 DEG C of ground；And/or
The processing time of the high-temperature process is 0.1-6h, preferably 0.3-4.5h, more preferably 0.5-4h.
In another preferred example, in step 2), the processing power of the supersound process is 80-320W, preferably 100-
250W, more preferably 120-200W；And/or
The processing time of the supersound process is 0.1-10h, preferably 0.3-6h, more preferably 0.5-3h.
In another preferred example, the aperture of filter screen used in the filtration treatment is 0.22-5um, preferably 0.4-
1um。
In another preferred example, the carrying out washing treatment is carried out using third solvent.
In another preferred example, the third solvent is water, preferably deionized water.
In another preferred example, in step 4), the centrifugal speed of the centrifugal treating is 500-8000rpm, preferably
800-6000rpm, more preferably 900-5000rpm；And/or
The centrifugation time of the centrifugal treating is 1-60min, preferably 3-30min, more preferably 5-20min.
In another preferred example, in step 4), the treatment temperature of the drying process is 50-120 DEG C, preferably 60-
90 DEG C, more preferably 80 DEG C；And/or
The processing time of the drying process is 0.5-4h, preferably 1-3h, more preferably 2h.
In another preferred example, yield >=10% of the method, preferably >=13%, more preferably >=16%, most preferably
>=18%.
The second aspect of the present invention, provides a kind of hexagonal boron nitride nanosheet, and the hexagonal boron nitride nanosheet is to adopt
It is prepared with the method described in first aspect present invention.
In another preferred example, the hexagonal boron nitride nanosheet has one or more features selected from the group below：
1) grain size of the hexagonal boron nitride nanosheet is 0.5-2.5um；
2) thickness of the hexagonal boron nitride nanosheet is 0.5-7nm；
3) surface modification of the hexagonal boron nitride nanosheet has hydroxyl；
4) 58W/mK is up to even backing thermal conductivity made of the hexagonal boron nitride nanosheet pumping rate.
It should be understood that within the scope of the present invention, above-mentioned each technical characteristic of the invention and have in below (eg embodiment)
It can be combined with each other between each technical characteristic of body description, to form a new or preferred technical solution.As space is limited, exist
This no longer tires out one by one states.
Description of the drawings
Fig. 1 is the SEM results of 1 gained hexagonal boron nitride nanosheet of embodiment.
Fig. 2 is the TEM results of 1 gained hexagonal boron nitride nanosheet of embodiment.
Fig. 3 is the FT-IR results of 1 gained hexagonal boron nitride nanosheet of raw material hexagonal boron nitride powder and embodiment.
Fig. 4 is the dispersed test result of 1 gained hexagonal boron nitride nanosheet of embodiment.
Specific implementation mode
The present inventor's in-depth study by long-term pre-processes hexagonal boron nitride powder by using molten caustic soda intercalation,
Hexagonal boron nitride nanosheet can expeditiously be made in a relatively short period of time in conjunction with ultrasonic lift-off technology.On this basis, it invents
People completes the present invention.
Term
As used herein, term " molten caustic soda " refers to the alkali melted through high-temperature process, the treatment temperature of the high-temperature process
Generally 100-300 DEG C, the processing time of the high-temperature process is generally 0.1-5h, and the alkali is preferably object selected from the group below
Matter：Sodium hydroxide, potassium hydroxide, or combinations thereof.
As used herein, term " ultrasound stripping ", which refers to the stripping, is realized by being ultrasonically treated.
Preparation method
The present invention provides a kind of methods preparing hexagonal boron nitride nanosheet, and described method includes following steps：
1) the first mixed liquor is provided, first mixed liquor includes the first solvent and is scattered among first solvent
Through the pretreated hexagonal boron nitride powder of molten caustic soda；
2) it is ultrasonically treated first mixed liquor, obtains the second mixed liquor；
3) optionally the second mixed liquor described in filtration treatment, and precipitation obtained by carrying out washing treatment, and products therefrom is disperseed again
In the second solvent, third mixed liquor is obtained；
4) centrifugal treating abovementioned steps products therefrom, collects upper layer dispersion liquid, and drying process obtains hexagonal nanometer boron nitride
Piece.
In another preferred example, first solvent and second solvent are water, preferably deionized water.
In another preferred example, after step 4), following steps are also optionally included：
5) centrifugation gained sediment in step 4) is scattered in again in the second solvent, adds alkaline matter, it is mixed obtains the 4th
Close liquid；
6) step 2) -4 is repeated), difference is：First mixed liquor is replaced with the 4th mixed liquor.
In another preferred example, step 5) -6 is repeated), it is preferable that number of repetition is 1-5 times.
In the present invention, described to be prepared as follows through the pretreated hexagonal boron nitride powder of molten caustic soda：
A-1) alkaline matter and hexagonal boron nitride powder are provided；
A-2 the alkaline matter and the hexagonal boron nitride powder) are mixed, the first mixture is obtained；
A-3) the first mixture described in high-temperature process obtains described through the pretreated hexagonal boron nitride powder of molten caustic soda.
In another preferred example, the grain size of the hexagonal boron nitride powder is 1-20 μm, preferably 3-18 μm, more preferably 4-
15μm。
In the present invention, the alkaline matter includes (but being not limited to)：Sodium hydroxide, potassium hydroxide, or combinations thereof.
In another preferred example, the alkaline matter is the mixture of sodium hydroxide and potassium hydroxide.
In another preferred example, in the alkaline matter, the mass mixing ratio of sodium hydroxide and potassium hydroxide is 0.1-5,
Preferably 0.3-3, more preferably 0.5-2.5.
In the present invention, in first mixture, the mass ratio of the alkaline matter and the hexagonal boron nitride powder
For 1-20, preferably 1-10, more preferably 1-6.
In the present invention, the treatment temperature of the high-temperature process be 100-300 DEG C, preferably 120-260 DEG C, more preferably
140-240℃；And/or
The processing time of the high-temperature process is 0.1-6h, preferably 0.3-4.5h, more preferably 0.5-4h.
In the present invention, in step 2), the processing power of the supersound process is 80-320W, preferably 100-250W, more
Good ground 120-200W；And/or
The processing time of the supersound process is 0.1-10h, preferably 0.3-6h, more preferably 0.5-3h.
In another preferred example, the aperture of filter screen used in the filtration treatment is 0.22-5um, preferably 0.4-
1um。
In another preferred example, the carrying out washing treatment is carried out using third solvent.
In another preferred example, the third solvent is water, preferably deionized water.
In the present invention, in step 4), the centrifugal speed of the centrifugal treating is 500-8000rpm, preferably 800-
6000rpm, more preferably 900-5000rpm；And/or
The centrifugation time of the centrifugal treating is 1-60min, preferably 3-30min, more preferably 5-20min.
In the present invention, in step 4), the treatment temperature of the drying process is 50-120 DEG C, preferably 60-90 DEG C,
More preferably 80 DEG C；And/or
The processing time of the drying process is 0.5-4h, preferably 1-3h, more preferably 2h.
In another preferred example, yield >=10% of the method, preferably >=13%, more preferably >=16%, most preferably
>=18%.
Typically, the preparation method includes the following steps：
1) sodium hydroxide and potassium hydroxide are milled and is stirred into mixed alkali, then again by mixed alkali and hexagonal boron nitride powder
It is uniformly mixed resulting mixture；
2) mixture of preparation is transferred to polytetrafluoroethylene (PTFE) crucible and be put into autoclave, carry out reaction 1 at high temperature
Cooled to room temperature after~5h；
3) gained reactant is scattered in ultrasound stripping in deionized water, then product filtering will be obtained, be washed with deionized water
It is centrifuged after being scattered in again in deionized water after washing, is dried to get to the hexagonal boron nitride after collecting upper layer dispersion liquid
Nanometer sheet；
4) centrifugal sediment obtained by above-mentioned steps is scattered in deionized water, sodium hydroxide is added and is carried out with potassium hydroxide
Ultrasound stripping, then product filtering will be obtained, it is washed with deionized, is centrifuged after disperseing again, after collecting upper layer dispersion liquid
It is dry, that is, obtain the hexagonal boron nitride nanosheet；
5) it optionally repeats step 4) and further increases stripping yield.
The average diameter for the hexagonal boron nitride powder that the present invention uses is 3~15 μm.Hexagonal boron nitride powder and molten caustic soda
The optimization time of reaction is 1~5h.
In the present invention, we pre-process the hexagonal boron nitride powder first with molten caustic soda intercalation, then will locate in advance again
The boron nitride powder managed carries out ultrasonic stripping in aqueous slkali, so as to obtain higher six sides nitrogen in a relatively short period of time
Change boron nanometer sheet (h-BNNs) yield.
This method has carried out functionalization while removing hexagonal boron nitride nanosheet (h-BNNs) in its sheet surfaces, greatly
It is big to improve the dispersibilities of h-BNNs in a solvent, and provide advantageous platform to be further surface-functionalized.
Hexagonal boron nitride nanosheet
The present invention provides a kind of hexagonal boron nitride nanosheet, the hexagonal boron nitride nanosheet is to use the method
It prepares.
In the present invention, the hexagonal boron nitride nanosheet has one or more features selected from the group below：
1) grain size of the hexagonal boron nitride nanosheet is 0.5-2.5um；
2) thickness of the hexagonal boron nitride nanosheet is 0.5-7nm；
3) surface modification of the hexagonal boron nitride nanosheet has hydroxyl；
4) 58W/mK is up to even backing thermal conductivity made of the hexagonal boron nitride nanosheet pumping rate.
Compared with prior art, the present invention has following major advantage：
(1) preparation method have it is simple for process, processing raw material it is cheap and easy to get, it is low for equipment requirements, to environmental toxicity
It is small and convenient for large-scale production the characteristics of, the cost of product can be substantially reduced；
(2) preparation method has the characteristics that rapidly and efficiently, yield is up to 19%；
(3) the hexagonal boron nitride nanosheet size is 0.5-2.5um, and thickness is 0.5-7nm.
(4) there is hydroxyl modified on the hexagonal boron nitride nanosheet surface, is easy to twice dispersing in deionized water；
(5) thermal conductivity is up to 58W/ in the face of the even backing of boron nitride made of the hexagonal boron nitride nanosheet pumping rate
mK。
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In the following examples, the experimental methods for specific conditions are not specified, usually according to conventional strip
Part or according to the normal condition proposed by manufacturer.Unless otherwise stated, otherwise percentage and number are calculated by weight.
Unless otherwise defined, all professional and scientific terms used in text and meaning known to one skilled in the art
Justice is identical.In addition, any method and material similar or impartial to described content can be applied to the method for the present invention.Wen Zhong
The preferred implement methods and materials are for illustrative purposes only.
Embodiment 1
(1) sodium hydroxide and potassium hydroxide 2.5g are weighed respectively, are fully milled and are mixed into mixed alkali, then again mix this
Alkali and 5g hexagonal boron nitride powders (grain size is about 3-18um) are uniformly mixed.
(2) gained mixture is transferred to polytetrafluoroethylene (PTFE) crucible and be put into autoclave, nature after 1h is reacted at 180 DEG C
It is cooled to room temperature.
(3) reaction product in reaction kettle is scattered in deionized water, gained mixed liquor is subjected to 160W ultrasound strippings
After ultrasonic, gained mixture is filtered (aperture of filter screen is 0.4um) by 1h, anti-with 90 DEG C of ionized waters in room temperature
After backwashing is for several times so as to by lye and boric acid object (mixture of such as Boratex and potassium borate) wash clean.After cleaning product, by gained
Product is centrifuged (centrifugal speed is 1700 revs/min, centrifugation time 30min) after being scattered in again in deionized water, collected
(it is 80 DEG C to be dried temperature, processing time 2h) dry after the dispersion liquid of upper layer.
(4) precipitation of centrifugation gained in above-mentioned steps is scattered in deionized water again, sodium hydroxide and hydrogen-oxygen is added
Change each 2.5g of potassium.Mixed liquor is subjected to 160W ultrasounds and removes 1h.After ultrasound, gained mixture is filtered, in room temperature
It is washed repeatedly for several times so as to by lye and borate wash clean with 90 DEG C of ionized waters.After cleaning product, product is disperseed again laggard
Drying after the dispersion liquid of upper layer is collected in row centrifugation, and gained is hexagonal boron nitride nanosheet, yield 13%.
As a result
SEM, TEM, FT-IR and dispersibility test are carried out respectively to 1 gained hexagonal boron nitride nanosheet of embodiment.
Fig. 1 is the SEM results of 1 gained hexagonal boron nitride nanosheet of embodiment.
As can be seen from Figure 1：Gained hexagonal boron nitride nanosheet size is 0.5-2.5um, and thickness is about 0.5-7nm.
Fig. 2 is the TEM results of 1 gained hexagonal boron nitride nanosheet of embodiment.
As can be seen from Figure 2：Hexagonal boron nitride powder is successfully removed into hexagonal boron nitride nanosheet.
Fig. 3 is 1 gained hexagonal boron nitride nanosheet (h-BNNS) of raw material hexagonal boron nitride powder (h-BN) and embodiment
FT-IR results.
As can be seen from Figure 3：Gained hexagonal boron nitride nanosheet surface modification has hydroxyl.
Fig. 4 is the dispersed test result of 1 gained hexagonal boron nitride nanosheet of embodiment.
As can be seen from Figure 4：Gained hexagonal boron nitride nanosheet again ultrasonic disperse is stood in deionized water after 16h without bright
Aobvious sedimentation.
Embodiment 2
With embodiment 1, difference lies in：In step (1) and (4) addition of sodium hydroxide and potassium hydroxide be respectively 3g and
2g。
Embodiment 3
With embodiment 1, difference lies in：The addition of sodium hydroxide and potassium hydroxide is respectively in step (1) and (4)
3.33g and 1.67g.
Embodiment 4
With embodiment 1, difference lies in：The addition of hexagonal boron nitride powder is 2g in step (1).
Embodiment 5
With embodiment 1, difference lies in：The addition of hexagonal boron nitride powder is 1g in step (1).
Embodiment 6
With embodiment 1, difference lies in：Reaction temperature in step (2) is 150 DEG C.
Embodiment 7
With embodiment 1, difference lies in：Reaction temperature in step (2) is 200 DEG C.
Embodiment 8
With embodiment 1, difference lies in：It is reacted at 180 DEG C in step (2), reaction time 2h.
Embodiment 9
With embodiment 1, difference lies in：It is reacted at 180 DEG C in step (2), reaction time 4h.
Embodiment 10
With embodiment 1, difference lies in：After step (4), the precipitation of centrifugation gained is scattered in deionized water again
In, sodium hydroxide 2.16g and potassium hydroxide 2.84g is added.Gained mixed liquor is subjected to ultrasound stripping 2h.It, will after ultrasound
Gained mixture is filtered, and is washed repeatedly for several times so as to by lye and borate wash clean with 90 DEG C of ionized waters in room temperature.It cleans
It after product, is centrifuged after product is disperseed again, collects drying after the dispersion liquid of upper layer, gained is hexagonal nanometer boron nitride
Piece, yield are 16.5% (1 product of cumulative embodiment).
Embodiment 11
With embodiment 10, difference lies in：After embodiment 10, the precipitation of centrifugation gained is scattered in 250mL again
In ionized water, sodium hydroxide 2.156g and potassium hydroxide 2.844g is added.Gained mixed liquor is subjected to ultrasound stripping 2h.Ultrasound knot
Gained mixture is filtered by Shu Hou, is washed repeatedly with 90 DEG C of ionized waters in room temperature dry to wash lye and borate for several times
Only.It after cleaning product, is centrifuged after products therefrom is scattered in again in deionized water, collects drying after the dispersion liquid of upper layer,
Gained is also hexagonal boron nitride nanosheet, and yield is 18.2% (10 product of cumulative embodiment).
Embodiment 12
With embodiment 11, difference lies in：After embodiment 11, the precipitation of centrifugation gained is scattered in 250mL again
In ionized water, sodium hydroxide 2.156g and potassium hydroxide 2.844g is added.Gained mixed liquor is subjected to ultrasound stripping 2h.Ultrasound knot
Gained mixture is filtered by Shu Hou, is washed repeatedly with 90 DEG C of ionized waters in room temperature dry to wash lye and borate for several times
Only.It after cleaning product, is centrifuged after products therefrom is disperseed again, collects drying after the dispersion liquid of upper layer, gained is also six sides
Boron nitride nanosheet, yield are 19% (11 product of cumulative embodiment).
The testing result of hexagonal boron nitride nanosheet and 1 gained hexagonal boron nitride nanosheet of embodiment obtained by embodiment 2-12
Testing result it is similar.
Embodiment 13
Even backing, gained are prepared using conventional method with any gained hexagonal boron nitride nanosheets of 1-12 of the embodiment of the present invention
The thermal conductivity of even backing is up to 58W/mK.
All references mentioned in the present invention is incorporated herein by reference, independent just as each document
It is incorporated as with reference to such.In addition, it should also be understood that, after reading the above teachings of the present invention, those skilled in the art can
To be made various changes or modifications to the present invention, such equivalent forms equally fall within model defined by the application the appended claims
It encloses.
Claims (10)
1. a kind of method preparing hexagonal boron nitride nanosheet, which is characterized in that described method includes following steps：
1) the first mixed liquor is provided, first mixed liquor includes that the first solvent and the warp being scattered among first solvent are molten
Melt the hexagonal boron nitride powder of oxygenation pretreatment；
2) it is ultrasonically treated first mixed liquor, obtains the second mixed liquor；
3) optionally the second mixed liquor described in filtration treatment, and precipitation obtained by carrying out washing treatment, and products therefrom is scattered in the again
In two solvents, third mixed liquor is obtained；
4) centrifugal treating abovementioned steps products therefrom, collects upper layer dispersion liquid, and drying process obtains hexagonal boron nitride nanosheet.
2. the method as described in claim 1, which is characterized in that it is described through the pretreated hexagonal boron nitride powder of molten caustic soda be as
Lower preparation：
A-1) alkaline matter and hexagonal boron nitride powder are provided；
A-2 the alkaline matter and the hexagonal boron nitride powder) are mixed, the first mixture is obtained；
A-3) the first mixture described in high-temperature process obtains described through the pretreated hexagonal boron nitride powder of molten caustic soda.
3. method as claimed in claim 2, which is characterized in that the alkaline matter is selected from the group：Sodium hydroxide, hydroxide
Potassium, or combinations thereof.
4. method as claimed in claim 2, which is characterized in that in first mixture, the alkaline matter and described six
The mass ratio of square boron nitride powder is 1-20.
5. method as claimed in claim 2, which is characterized in that the treatment temperature of the high-temperature process is 100-300 DEG C；With/
Or
The processing time of the high-temperature process is 0.1-6h.
6. the method as described in claim 1, which is characterized in that in step 2), the processing power of the supersound process is 80-
320W；And/or
The processing time of the supersound process is 0.1-10h.
7. the method as described in claim 1, which is characterized in that in step 4), the centrifugal speed of the centrifugal treating is 500-
8000rpm；And/or
The centrifugation time of the centrifugal treating is 1-60min.
8. the method as described in claim 1, which is characterized in that in step 4), the treatment temperature of the drying process is 50-
120℃；And/or
The processing time of the drying process is 0.5-4h.
9. a kind of hexagonal boron nitride nanosheet, which is characterized in that the hexagonal boron nitride nanosheet is using described in claim 1
Method prepare.
10. hexagonal boron nitride nanosheet as claimed in claim 9, which is characterized in that the hexagonal boron nitride nanosheet has
One or more features selected from the group below：
1) grain size of the hexagonal boron nitride nanosheet is 0.5-2.5um；
2) thickness of the hexagonal boron nitride nanosheet is 0.5-7nm；
3) surface modification of the hexagonal boron nitride nanosheet has hydroxyl；
4) 58W/mK is up to even backing thermal conductivity made of the hexagonal boron nitride nanosheet pumping rate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710128745.XA CN108529573B (en) | 2017-03-06 | 2017-03-06 | Method for preparing hexagonal boron nitride nanosheets by using molten alkali and ultrasonic stripping technology |
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| CN201710128745.XA CN108529573B (en) | 2017-03-06 | 2017-03-06 | Method for preparing hexagonal boron nitride nanosheets by using molten alkali and ultrasonic stripping technology |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111717900A (en) * | 2020-07-06 | 2020-09-29 | 河北工业大学 | Mechanical stripping method of functionalized boron nitride nanosheets |
| CN111733401A (en) * | 2020-06-18 | 2020-10-02 | 浙江大学 | Preparation method of high-thermal-conductivity inorganic lead-halogen perovskite composite film |
| CN112538284A (en) * | 2020-12-16 | 2021-03-23 | 齐鲁工业大学 | Glass bottle hot end spraying liquid and preparation method thereof |
| CN116178642A (en) * | 2023-04-24 | 2023-05-30 | 山东鹏程陶瓷新材料科技有限公司 | Surface grafting modified hexagonal boron nitride and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8303922B2 (en) * | 2009-08-24 | 2012-11-06 | The United States Of America As Represeted By The Administrator Of The National Aeronautics And Space Administration | Method for exfoliation of hexagonal boron nitride |
| CN102976295A (en) * | 2012-12-27 | 2013-03-20 | 山东大学 | Method for preparing two-dimensional hexagonal boron nitride nanosheet through molten caustic soda |
| US20140077138A1 (en) * | 2012-09-10 | 2014-03-20 | William Marsh Rice University | Boron nitride-based fluid compositions and methods of making the same |
| CN104085882A (en) * | 2014-06-24 | 2014-10-08 | 华南理工大学 | Preparation method of few-layer oxygen-containing fluorinated graphene |
| CN104944392A (en) * | 2014-03-25 | 2015-09-30 | 中国科学院大连化学物理研究所 | Mass preparation method of graphite-phase carbon nitride nanosheets |
| KR20160125711A (en) * | 2015-04-22 | 2016-11-01 | 한국과학기술원 | Method of manufacturing high-quality hexaganal boron nitride nanosheets and hexagonal boron nitride nanosheets manufactured by using the method thereof |
-
2017
- 2017-03-06 CN CN201710128745.XA patent/CN108529573B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8303922B2 (en) * | 2009-08-24 | 2012-11-06 | The United States Of America As Represeted By The Administrator Of The National Aeronautics And Space Administration | Method for exfoliation of hexagonal boron nitride |
| US20140077138A1 (en) * | 2012-09-10 | 2014-03-20 | William Marsh Rice University | Boron nitride-based fluid compositions and methods of making the same |
| CN102976295A (en) * | 2012-12-27 | 2013-03-20 | 山东大学 | Method for preparing two-dimensional hexagonal boron nitride nanosheet through molten caustic soda |
| CN104944392A (en) * | 2014-03-25 | 2015-09-30 | 中国科学院大连化学物理研究所 | Mass preparation method of graphite-phase carbon nitride nanosheets |
| CN104085882A (en) * | 2014-06-24 | 2014-10-08 | 华南理工大学 | Preparation method of few-layer oxygen-containing fluorinated graphene |
| KR20160125711A (en) * | 2015-04-22 | 2016-11-01 | 한국과학기술원 | Method of manufacturing high-quality hexaganal boron nitride nanosheets and hexagonal boron nitride nanosheets manufactured by using the method thereof |
Non-Patent Citations (3)
| Title |
|---|
| LI FU ET AL: "In situ growth of metal nanoparticles on boron nitride nanosheets as highly efficient catalysts", 《J. MATER. CHEM. A》 * |
| LI, XIANLEI ET AL: "Exfoliation of Hexagonal Boron Nitride by Molten Hydroxides", 《ADVANCED MATERIALS》 * |
| 王婷 等: "石墨烯/氮化硼/石墨烯三明治薄膜的制备和导热性能", 《热加工工艺》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111733401A (en) * | 2020-06-18 | 2020-10-02 | 浙江大学 | Preparation method of high-thermal-conductivity inorganic lead-halogen perovskite composite film |
| CN111733401B (en) * | 2020-06-18 | 2021-10-22 | 浙江大学 | Preparation method of high-thermal-conductivity inorganic lead-halogen perovskite composite film |
| CN111717900A (en) * | 2020-07-06 | 2020-09-29 | 河北工业大学 | Mechanical stripping method of functionalized boron nitride nanosheets |
| CN111717900B (en) * | 2020-07-06 | 2021-11-23 | 河北工业大学 | Mechanical stripping method of functionalized boron nitride nanosheets |
| CN112538284A (en) * | 2020-12-16 | 2021-03-23 | 齐鲁工业大学 | Glass bottle hot end spraying liquid and preparation method thereof |
| CN116178642A (en) * | 2023-04-24 | 2023-05-30 | 山东鹏程陶瓷新材料科技有限公司 | Surface grafting modified hexagonal boron nitride and preparation method thereof |
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