CN104803363A - Method for preparing hexagonal boron nitride nanosheets massively - Google Patents
Method for preparing hexagonal boron nitride nanosheets massively Download PDFInfo
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- CN104803363A CN104803363A CN201510174176.3A CN201510174176A CN104803363A CN 104803363 A CN104803363 A CN 104803363A CN 201510174176 A CN201510174176 A CN 201510174176A CN 104803363 A CN104803363 A CN 104803363A
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Abstract
The invention relates to a method for preparing hexagonal boron nitride nanosheets massively, and belongs to the technical field of functional materials. According to the method, a high cut dispersion emulsification machine is used for cutting and stripping hexagonal boron nitride to realize efficient stripping of hexagonal boron nitride; a product is centrifuged, filtered and dried to obtain single-layer or few-layer hexagonal boron nitride nanosheets. The hexagonal boron nitride nanosheets prepared with the method are high in purity and integral in structure. The method has the advantages of simplicity in operation, safety, low cost and the like, and is suitable for preparing high-quality hexagonal boron nitride nanosheets.
Description
Technical field
The present invention relates to a kind of method preparing hexagonal boron nitride nanosheet in enormous quantities, belong to technical field of function materials.
Background technology
Boron nitride (BN) has good oxidation-resistance, electrical insulating property, erosion resistance, and have the multiple crystal formations such as amorphous, cubic nonlinearity six side, wherein, six square boron nitride have the laminate structure being similar to graphite, therefore chemical property is the most stable.Hexagonal boron nitride is one of material that in stupalith, heat conduction is maximum; The coefficient of expansion is equivalent to quartz, is minimum in pottery, so thermal shock resistance is fine.After the research of Graphene in 2010 obtains Nobel Prize in physics, the research about Graphene gets more and more, the electronics of individual layer hexagonal boron nitride and crystalline network and Graphene closely, so be referred to as again " white graphite alkene ".The thermal conductivity of single-layer silicon nitride boron or boron nitride nanosheet (f-hBN) is very high (300 ~ 2000 W/mk), and has good electrical insulating property (10
4cm), high thermal resistance (oxidation resistance temperature 900 DEG C), low thermal coefficient of expansion (10
-6, be only second to quartz), soft (Mohs' hardness 2), the performance characteristics such as chemical resistance, self lubricity.
Boron nitride nanosheet has many preparation methods.Ball milling, the mechanically peel method productive rate such as ultrasonic are very low; The boron nitride nanometer chip size that liquid phase stripping method obtains is less, and aftertreatment bothers; Vapour deposition process appointed condition is harsh, and experimentation is difficult to control, and toxicity is very large and output is lower, cost is higher, is difficult to large-scale production.Chinese patent CN 102887490 A discloses a kind of method of ultrasonic stripping individual layer or few layer hexagonal boron nitride, the method needs boron nitride and organic solvent to stir 20-30h at 45 ~ 55 DEG C of lower magnetic forces, ultrasonic 20h after being cooled to room temperature, then 1-3 days is left standstill, production cycle is very long, is not suitable for producing in enormous quantities.Chinese patent CN 103626141 A discloses a kind of method utilizing chemical stripping to prepare hexagonal boron nitride nanosheet, and the phase needs acidic solution to be washed to repeatedly PH between 6 ~ 8 the method after the reaction, and last handling process is more loaded down with trivial details.Chinese patent CN 103570003 discloses a kind of method that ball milling peels off Graphene and two-dimentional boron nitride crystal material, show according to appended SEM figure, the thickness of the boron nitride nanosheet that the method obtains is greater than 5 nm, the number of plies of boron nitride is more, and therefore the boron nitride nanometer tablet quality prepared of the method is lower.
Summary of the invention
The object of the invention is to overcome the deficiency that current existing preparation method exists, provide that a kind of cost is low, technique simple, be easy to the mass-produced method preparing boron nitride nanosheet, effectively improve preparation efficiency and the quality of stone boron nitride nanosheet.
A kind of method preparing hexagonal boron nitride nanosheet in enormous quantities of the present invention, is characterized in that having following process and step:
By hexagonal boron nitride powder and polar organic solvent mixing and stirring by a certain percentage, carry out shearing by high-shearing dispersion emulsifying machine and peel off.Control certain velocity of shear and shear time.Then mixed solution is carried out centrifugal, collect supernatant liquor carry out filtering, dry, finally obtain hexagonal boron nitride nanosheet.
Described solvent is any one in dodecyl pyrrolidone, Virahol, N-Methyl pyrrolidone, dimethyl formamide, N-METHYLFORMAMIDE;
Described organic solvent and the ratio of powder are at 20:1 ~ 80:1;
Described shearing exfoliation temperature is at 20 ~ 40 DEG C, and splitting time is 30 ~ 120 minutes;
The rotating speed that described shearing is peeled off is at 7200 ~ 16000 RPM;
The bore dia of filtering membrane of the present invention is at 0.01 ~ 0.5 mm.
The selection condition of solvent for use of the present invention: 1. peel off and centrifugal after, the BN stabilizing dissolved that is stripped can be made or to suspend and in solution; 2. the extent of exfoliation of BN is higher.
The surface tension of organic solvent has important impact to peeling effect.Surface tension 40 ~ 50 mN/m of selected organic solvent.
Compared with prior art, the present invention has following features.
(1) this invention exploits a kind of new technology route sheared stripping hexagonal boron nitride and prepare hexagonal boron nitride nanosheet, this technique preparation cost is low, easy to control, can realize industrial mass production.
(2) the object product hexagonal boron nitride nanosheet prepared of the present invention, the thickness of boron nitride nanosheet is between 1 ~ 5 nm, and width is between 1-5 mm.Its purity is high, and defect is few, and foreign matter content is low, good dispersity.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of preparation hexagonal boron nitride nanosheet.
Fig. 2 is the photo of hexagonal boron nitride nanosheet dispersion liquid and untreated hexagonal boron nitride.
Fig. 3 is the photo that the Tyndall phenomenon of hexagonal boron nitride nanosheet dispersion liquid and untreated hexagonal boron nitride contrasts.(generation due to Tyndall phenomenon requires that the radius of dispersate particle is between 1nm to visible wavelength range, therefore can prove to obtain nano level boron nitride sheet at macroscopic perspective.）
Fig. 4 is the hexagonal boron nitride nanosheet Tyndall phenomenon figure of different organic solvents.
The high-resolution-ration transmission electric-lens photo of the hexagonal boron nitride nanosheet of Fig. 5 prepared by the embodiment of the present invention 1.
The high-resolution-ration transmission electric-lens photo of the hexagonal boron nitride nanosheet of Fig. 6 prepared by the embodiment of the present invention 1.
The high-resolution-ration transmission electric-lens photo of the hexagonal boron nitride nanosheet of Fig. 7 prepared by the embodiment of the present invention 3.
The high-resolution-ration transmission electric-lens photo of the hexagonal boron nitride nanosheet of Fig. 8 prepared by the embodiment of the present invention 3.
The high-resolution-ration transmission electric-lens photo of the hexagonal boron nitride nanosheet of Fig. 9 prepared by the embodiment of the present invention 4.
The high-resolution-ration transmission electric-lens photo of the hexagonal boron nitride nanosheet of Figure 10 prepared by the embodiment of the present invention 4.
Embodiment
Below by specific embodiments and the drawings, the present invention is further described.
Embodiment 1
Take 5 g hexagonal boron nitrides respectively and 400 g Virahols are put in beaker, on high-shearing dispersion emulsifying machine, carry out shearing under 20 degrees Celsius peel off, the ratio shearing solvent and solid in stripping process is 80:1, the rotating speed of high-shearing dispersion emulsifying machine is 7200 revs/min, and shearing splitting time is 2 hours.The product obtained is carried out centrifugation, and centrifugation rotating speed is at 3000 RPM, and the centrifugation rotating speed time is 10 minutes.Collect supernatant liquor carry out filtering, dry, obtain hexagonal boron nitride nanosheet, the bore dia of filtering membrane is at 0.1 mm.
Embodiment 2
Take 10 g hexagonal boron nitrides respectively and 400 g Virahols are put in beaker, on high-shearing dispersion emulsifying machine, carry out shearing under 20 degrees Celsius peel off, the ratio shearing solvent and solid in stripping process is 40:1, the rotating speed of high-shearing dispersion emulsifying machine is 16000 revs/min, and shearing splitting time is 2 hours.The product obtained is carried out centrifugation, and centrifugation rotating speed is at 3000 RPM, and the centrifugation rotating speed time is 10 minutes.Collect supernatant liquor carry out filtering, dry, obtain hexagonal boron nitride nanosheet, the bore dia of filtering membrane is at 0.1 mm.
Embodiment 3
Take 5 g hexagonal boron nitrides respectively and 400 g N-Methyl pyrrolidone are put in beaker, on high-shearing dispersion emulsifying machine, carry out shearing under 20 degrees Celsius peel off, the ratio shearing solvent and solid in stripping process is 80:1, the rotating speed of high-shearing dispersion emulsifying machine is 7200 revs/min, and shearing splitting time is 3 hours.The product obtained is carried out centrifugation, and centrifugation rotating speed is at 3000 RPM, and the centrifugation rotating speed time is 10 minutes.Collect supernatant liquor carry out filtering, dry, obtain hexagonal boron nitride nanosheet, the bore dia of filtering membrane is at 0.1 mm.
Embodiment 4
Take 10 g hexagonal boron nitrides respectively and 400 g dimethyl formamides are put in beaker, on high-shearing dispersion emulsifying machine, carry out shearing under 20 degrees Celsius peel off, the ratio shearing solvent and solid in stripping process is 40:1, the rotating speed of high-shearing dispersion emulsifying machine is 12000 revs/min, and shearing splitting time is 2 hours.The product obtained is carried out centrifugation, and centrifugation rotating speed is at 3000 RPM, and the centrifugation rotating speed time is 10 minutes.Collect supernatant liquor carry out filtering, dry, obtain hexagonal boron nitride nanosheet, the bore dia of filtering membrane is at 0.1 mm.
Claims (1)
1. prepare a method for hexagonal boron nitride nanosheet in enormous quantities, it is characterized in that there is following process and step:
A, by hexagonal boron nitride powder and polar organic solvent mixing and stirring by a certain percentage, described polar organic solvent is any one in dodecyl pyrrolidone, Virahol, N-Methyl pyrrolidone, dimethyl formamide, N-METHYLFORMAMIDE; Described organic solvent and the ratio of hexagonal boron nitride powder are at 20:1 ~ 80:1;
B, to be carried out shearing peel off by high-shearing dispersion emulsifying machine under certain temperature, velocity of shear and shear time, described shearing exfoliation temperature is at 20 ~ 40 DEG C, and splitting time is 30 ~ 120 minutes, shears the rotating speed peeled off at 7200 ~ 16000 RPM;
C, mixed solution is carried out centrifugal, collect supernatant liquor carry out filtering, dry, finally obtain hexagonal boron nitride nanosheet.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105524617A (en) * | 2015-12-21 | 2016-04-27 | 东南大学 | Preparation method of molybdenum selenide quantum dots |
| CN106281126A (en) * | 2016-08-31 | 2017-01-04 | 广东纳路纳米科技有限公司 | Double glazing modified white graphite alkene composite butyl fluid sealant and encapsulating method thereof |
| CN107244659A (en) * | 2017-05-11 | 2017-10-13 | 中国科学院山西煤炭化学研究所 | A kind of liquid phase shearing prepares the brilliant method of monodisperse colloid boron nitride nanometer |
| CN107416780A (en) * | 2017-09-21 | 2017-12-01 | 湖北科技学院 | A kind of preparation method of few layer hexagonal boron nitride |
| CN108033442A (en) * | 2016-12-12 | 2018-05-15 | 广东纳路纳米科技有限公司 | A kind of method that high speed peels off white graphite alkene |
| CN108165342A (en) * | 2018-02-22 | 2018-06-15 | 大连圣多教育咨询有限公司 | A kind of self-restoring lubricating oil and preparation method |
| CN108165343A (en) * | 2018-02-22 | 2018-06-15 | 大连圣多教育咨询有限公司 | A kind of self-restoring lubricating oil additive and preparation method |
| CN108529575A (en) * | 2018-07-16 | 2018-09-14 | 齐鲁师范学院 | A method of preparing boron nitride nanosheet using solvent thermal reaction |
| CN109353997A (en) * | 2018-11-15 | 2019-02-19 | 中国科学院兰州化学物理研究所 | A kind of method that magnanimity prepares hexagonal nanometer boron nitride volume |
| CN109385322A (en) * | 2018-10-24 | 2019-02-26 | 中国科学院兰州化学物理研究所 | A kind of preparation method of ultra-low friction hexagonal boron nitride fluid lubricant |
| CN109704770A (en) * | 2019-01-29 | 2019-05-03 | 齐鲁工业大学 | Add the self-lubrication ceramic cutter material and preparation method thereof of nickel coated hexagonal boron nitride nanosheet composite granule |
| CN111115591A (en) * | 2020-01-03 | 2020-05-08 | 青岛科技大学 | Ultra-high concentration boron nitride nano paste and preparation method thereof |
| CN112142019A (en) * | 2020-09-28 | 2020-12-29 | 山东晶亿新材料有限公司 | Preparation method of hexagonal boron nitride nanosheet |
| CN113179611A (en) * | 2021-03-15 | 2021-07-27 | 佛山市晟鹏科技有限公司 | Boron nitride heat dissipation film and preparation method and application thereof |
| CN114891255A (en) * | 2022-05-27 | 2022-08-12 | 重庆大学 | Glass fiber reinforced hexagonal boron nitride three-dimensional ordered framework composite epoxy resin and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105524617A (en) * | 2015-12-21 | 2016-04-27 | 东南大学 | Preparation method of molybdenum selenide quantum dots |
| CN106281126A (en) * | 2016-08-31 | 2017-01-04 | 广东纳路纳米科技有限公司 | Double glazing modified white graphite alkene composite butyl fluid sealant and encapsulating method thereof |
| CN106281126B (en) * | 2016-08-31 | 2017-12-29 | 广东纳路纳米科技有限公司 | Double glazing modified white graphite alkene composite butyl fluid sealant and its encapsulating method |
| CN108033442A (en) * | 2016-12-12 | 2018-05-15 | 广东纳路纳米科技有限公司 | A kind of method that high speed peels off white graphite alkene |
| WO2018107794A1 (en) * | 2016-12-12 | 2018-06-21 | 广东纳路纳米科技有限公司 | Method for exfoliating hexagonal boron nitride (h-bn) by means of high speed dispersion |
| CN107244659A (en) * | 2017-05-11 | 2017-10-13 | 中国科学院山西煤炭化学研究所 | A kind of liquid phase shearing prepares the brilliant method of monodisperse colloid boron nitride nanometer |
| CN107416780A (en) * | 2017-09-21 | 2017-12-01 | 湖北科技学院 | A kind of preparation method of few layer hexagonal boron nitride |
| CN108165342A (en) * | 2018-02-22 | 2018-06-15 | 大连圣多教育咨询有限公司 | A kind of self-restoring lubricating oil and preparation method |
| CN108165343A (en) * | 2018-02-22 | 2018-06-15 | 大连圣多教育咨询有限公司 | A kind of self-restoring lubricating oil additive and preparation method |
| CN108529575A (en) * | 2018-07-16 | 2018-09-14 | 齐鲁师范学院 | A method of preparing boron nitride nanosheet using solvent thermal reaction |
| CN109385322A (en) * | 2018-10-24 | 2019-02-26 | 中国科学院兰州化学物理研究所 | A kind of preparation method of ultra-low friction hexagonal boron nitride fluid lubricant |
| CN109353997A (en) * | 2018-11-15 | 2019-02-19 | 中国科学院兰州化学物理研究所 | A kind of method that magnanimity prepares hexagonal nanometer boron nitride volume |
| CN109353997B (en) * | 2018-11-15 | 2022-02-08 | 中国科学院兰州化学物理研究所 | Method for macroscopic quantity preparation of hexagonal boron nitride nano roll |
| CN109704770A (en) * | 2019-01-29 | 2019-05-03 | 齐鲁工业大学 | Add the self-lubrication ceramic cutter material and preparation method thereof of nickel coated hexagonal boron nitride nanosheet composite granule |
| CN109704770B (en) * | 2019-01-29 | 2021-10-22 | 齐鲁工业大学 | Self-lubricating ceramic cutting tool material added with nickel-coated hexagonal boron nitride nanosheet composite powder and preparation method thereof |
| CN111115591A (en) * | 2020-01-03 | 2020-05-08 | 青岛科技大学 | Ultra-high concentration boron nitride nano paste and preparation method thereof |
| CN112142019A (en) * | 2020-09-28 | 2020-12-29 | 山东晶亿新材料有限公司 | Preparation method of hexagonal boron nitride nanosheet |
| CN113179611A (en) * | 2021-03-15 | 2021-07-27 | 佛山市晟鹏科技有限公司 | Boron nitride heat dissipation film and preparation method and application thereof |
| CN113179611B (en) * | 2021-03-15 | 2023-03-24 | 佛山市晟鹏科技有限公司 | Boron nitride heat dissipation film and preparation method and application thereof |
| CN114891255A (en) * | 2022-05-27 | 2022-08-12 | 重庆大学 | Glass fiber reinforced hexagonal boron nitride three-dimensional ordered framework composite epoxy resin and preparation method and application thereof |
| CN114891255B (en) * | 2022-05-27 | 2023-08-18 | 重庆大学 | Glass fiber reinforced hexagonal boron nitride three-dimensional ordered frame composite epoxy resin and preparation method and application thereof |
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Application publication date: 20150729 |