CN107055561A - A kind of preparation method of boron alkene - Google Patents
A kind of preparation method of boron alkene Download PDFInfo
- Publication number
- CN107055561A CN107055561A CN201710313194.4A CN201710313194A CN107055561A CN 107055561 A CN107055561 A CN 107055561A CN 201710313194 A CN201710313194 A CN 201710313194A CN 107055561 A CN107055561 A CN 107055561A
- Authority
- CN
- China
- Prior art keywords
- boron
- hours
- ball
- preparation
- liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/023—Boron
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation method of boron alkene, its step is as follows：Boron source and catalyst are pressed 1:3~5 mass ratio carries out ball milling, and ratio of grinding media to material is 4~10:1, ball milling 40~60 hours cools down products therefrom 1~2 hour with liquid nitrogen immediately；Then by product separated 2~4 hours, remaining liquid borine is removed, then product is handled 2 hours with tube type vacuum stove, carbon impurity is removed；Products therefrom is subjected to liquid-solid extraction processing again, finally product is dried with vacuum drying chamber, room temperature is naturally cooled to, the boron alkene that purity is 95%~98.5% is obtained.Present device is simple, cost is relatively low, and products obtained therefrom purity is high, impurity is few, product quality is high, with promotional value.
Description
Technical field
The invention belongs to new material technology field, more particularly to a kind of preparation method of boron alkene.
Background of invention：
Graphene as the most thin, maximum intensity, electrical and thermal conductivity performance having now been found that a kind of most strong novel nano-material,
It is a kind of single layer of carbon atom structure in honeycomb arrangement, with excellent physical and chemical performance, has been widely used in super
The fields such as computer, photon sensor, gene sequencing, solar cell, therefore, graphene are referred to as " dark fund ", are " new materials
King ".
After graphene, scientist wishes to find more two-dimensional materials with good characteristic.Element boron is because being carbon
" neighbour " and as primary goal.However, it is referred to as the boron alkene of graphene " brother " not naturally occurring, can only be artificial synthesized.
Theoretical construct prediction of the scientist to boron alkene has exceeded 10 years as long as, but is synthesized from failed.Experimentally, due to boron be high-melting-point,
The material of low-steam pressure, it is extremely difficult that effective thermal evaporation temperature carries out thermal evaporation more than 2000 degrees Celsius, directly.Boron is prepared before this
Material mainly use boride, but be easy to introduce impurity, and chemical process is complicated.Even if there is the samples such as other film
It is successfully prepared, its structure is also complex.Therefore, the preparation of boron alkene turns into international condensed matter physics and Material Physics circle is generally acknowledged
World-famous puzzle.
2014, Nankai University School of Physics circumference cutting edge of a knife or a sword professor, Wang Huitian professors and Stony Brook University SUNY were difficult to understand
Professors Gan Nuofu etc. are based on evolution algorithm combination first-principles calculations, predict a unique two-dimentional boron structure.2015 7
Month, the research of boron alkene achieves breakthrough.U.S.'s Argonne National Laboratory, Nankai University, the New York State University's stone small stream point
The research unit such as school and Northwest University cooperates, and using the method for high vacuum atom sputtering, is successfully given birth on the surface of silver first
Grow the monoatomic layer boron alkene of fold.The experimental result that joint team obtains almost complies fully with [Yi Ming Sino-U.S. with theoretical model
Scientist, which cooperates to grind, obtains monoatomic thickness " boron alkene " [J] analysis test journals, 2016 (1):9-9.].The same period, Chinese Scientists
Also there is important breakthrough in the preparation of boron alkene.Inst. of Physics, CAS/Beijing condensed state National Laboratory (raises) table
Doctor Feng Baojie, Zhong Qing of Mian Shiwuke brightness seminar are under Wu Kehui researcher, the guidance of Chen Lan assistant researcher, using super
Hight atmospheric molecular beam epitaxy (MBE) directly carries out the method that monoatomic layer is constructed, and monolayer of boron is obtained on Ag (111) substrate
Alkene.They overcome the difficulty that boron is difficult to evaporate, using home made materials, have developed high-purity, the special graphite crucible of high temperature resistance.
Reuse electron beam heating crucible, realize direct thermal evaporation boron simple substance under ultra-high temperature [Liu Zhong models two dimension boron (boron alkene) into
Work(experiment obtains [J] Acta PhySico-Chimica Sinicas, 2016,32 (5):1053-1054.].
Although China and foreign countries scientist has been successfully prepared monolayer of boron alkene, it is due to that device therefor price is high, prepares bar
Part requires harsh, and chemical process is complicated, and production cost is higher, wants to prepare boron alkene on a large scale and be applied in practice still to have
Very big difficulty.So, the present invention proposes a kind of Novel boron alkene preparation method.
The content of the invention
It is an object of the invention to be to provide one kind, operation is simple, cost is relatively low, product purity is high, impurity is few, raw
Produce the preparation method of the boron alkene of efficiency high, it is to avoid existing methods critical conditions and complicated preparation process, and improve product matter
Amount.The present invention adds catalyst mainly using liquid borine as boron source, passes through ball milling, liquid nitrogen frozen, distillation, calcining and extraction
Take with drying process to prepare boron alkene.
Technical scheme is as follows：
(1) 1 is pressed:3~5 mass ratio, ball milling is carried out by boron source and catalyst, and ratio of grinding media to material is 4~10:1, abrading-ball is hard
Alloying pellet；The boron source is liquid borine, i.e. pentaborane or own borine；The catalyst be tungsten carbide powder, platinum powder or carbon dust and
Tungsten powder mass ratio is 1~1.3:10.21 mixture；
(2) raw material and abrading-ball are loaded into ball grinder in glove box, using high energy ball mill ball milling 40~60 hours, per ball
Mill stops 0.5 hour for 1 hour, and rotating speed is 400~600r/min；
(3) step (2) products therefrom is cooled down 1~2 hour with liquid nitrogen immediately；
(4) by the product separated 2~4 hours of step (3), remaining liquid borine is removed；
(5) step (4) products therefrom is handled 2 hours with tube type vacuum stove, removes carbon impurity；
(6) step (5) products therefrom is subjected to liquid-solid extraction processing, extractant is used as using ethanol (AR) or acetone (AR)；
(7) step (6) products therefrom is dried with vacuum drying chamber, temperature is 60~80 DEG C, the time is 10 hours,
Room temperature is naturally cooled to, the boron alkene that purity is 95~98.5% is obtained.
The present invention has the following advantages that compared with prior art：
(1) equipment is simple and safe, and operation is simple, and cost is relatively low.
(2) products obtained therefrom purity is high, and impurity is few, and quality is high.
(3) it can be mass, promotional value is high.
Embodiment
Embodiment 1：
Pentaborane 2g, tungsten carbide powder 6g, sintered carbide ball 32g are weighed with assay balance, by raw material and mill in glove box
Ball loads ball grinder, and using high energy ball mill ball milling 40 hours, drum's speed of rotation was 400r/min, and it is small to stop 0.5 within 1 hour per ball milling
When, after ball milling terminates, take out product；, will be surplus to product separated 2 hours after product is cooled down 1 hour with liquid nitrogen immediately
Extraction raffinate state borine is removed；Next product is handled 2 hours with tube type vacuum stove, removes carbon impurity；Then made with ethanol (AR)
For extractant, liquid-solid extraction processing is carried out to products therefrom；Finally product is dried 10 hours with vacuum drying chamber at 60 DEG C,
Room temperature is naturally cooled to, the boron alkene that purity is 95% is obtained.
Embodiment 2：
Pentaborane 2g, platinum powder 8g, sintered carbide ball 80g are weighed with assay balance, raw material and abrading-ball is filled in glove box
Enter ball grinder, using high energy ball mill ball milling 50 hours, drum's speed of rotation was 500r/min, stop within 1 hour 0.5 hour per ball milling,
After ball milling terminates, product is taken out；To product separated 3 hours after product is cooled down 1.5 hours with liquid nitrogen immediately, by raffinate
State borine is removed；Next product is handled 2 hours with tube type vacuum stove, removes carbon impurity；Then extraction is used as using ethanol (AR)
Agent is taken, liquid-solid extraction processing is carried out to products therefrom；Finally product is dried 10 hours with vacuum drying chamber at 70 DEG C, it is natural
Room temperature is cooled to, the boron alkene that purity is 97% is obtained.
Embodiment 3：
Pentaborane 2g, carbon dust 0.892g, tungsten powder 9.108g, sintered carbide ball 120g are weighed with assay balance, in glove box
Interior that raw material and abrading-ball are loaded into ball grinder, using high energy ball mill ball milling 60 hours, drum's speed of rotation was 600r/min, per ball milling
Stop within 1 hour 0.5 hour, after ball milling terminates, product is taken out in glove box；To production after product is cooled down 2 hours with liquid nitrogen immediately
Thing separated 4 hours, remaining liquid borine is removed；Next product is handled 2 hours with tube type vacuum stove, goes removal of impurities
Matter carbon；Then using acetone (AR) as extractant, liquid-solid extraction processing is carried out to products therefrom；It is finally dry with vacuum at 80 DEG C
Dry case is dried 10 hours to product, naturally cools to room temperature, obtains the boron alkene that purity is 98.5%.
Claims (4)
1. a kind of preparation method of boron alkene, it is characterised in that：It comprises the following steps：
(1) boron source and catalyst are pressed 1:3~5 mass ratio carries out ball milling, and ratio of grinding media to material is 4~10:1；
(2) raw material and abrading-ball are loaded into ball grinder under the atmosphere of glove box argon gas, it is small using high energy ball mill ball milling 40~60
When, stop within 1 hour 0.5 hour per ball milling, rotating speed is 400~600r/min；
(3) step (2) products therefrom is cooled down 1~2 hour with liquid nitrogen immediately；
(4) by the product separated 2~4 hours of step (3), remaining liquid borine is removed；
(5) step (4) products therefrom is handled 2 hours with tube type vacuum stove, removes carbon impurity；
(6) step (5) products therefrom is subjected to liquid-solid extraction processing, extractant is used as using ethanol (AR) or acetone (AR)；
(7) step (6) products therefrom is dried with vacuum drying chamber, temperature is 60~80 DEG C, the time is 10 hours, natural
Room temperature is cooled to, the boron alkene that purity is 95%~98.5% is obtained.
2. the preparation method of boron alkene according to claim 1, it is characterised in that：The boron source is liquid borine, i.e. pentaborane
Or own borine.
3. the preparation method of boron alkene according to claim 1, it is characterised in that：The catalyst be tungsten carbide powder, platinum powder or
Carbon dust and tungsten powder 1~1.3:10.21 mixture.
4. the preparation method of boron alkene according to claim 1, it is characterised in that：The abrading-ball is sintered carbide ball.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710313194.4A CN107055561B (en) | 2017-05-05 | 2017-05-05 | A kind of preparation method of boron alkene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710313194.4A CN107055561B (en) | 2017-05-05 | 2017-05-05 | A kind of preparation method of boron alkene |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107055561A true CN107055561A (en) | 2017-08-18 |
| CN107055561B CN107055561B (en) | 2018-12-28 |
Family
ID=59596032
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710313194.4A Active CN107055561B (en) | 2017-05-05 | 2017-05-05 | A kind of preparation method of boron alkene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107055561B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109149541A (en) * | 2018-09-16 | 2019-01-04 | 河南师范大学 | A kind of nanoscale demand limiter based on boron hydride alkene |
| CN109775710A (en) * | 2019-03-16 | 2019-05-21 | 南昌大学 | A kind of preparation method of nitrogen-doped porous carbon material and the application in supercapacitor |
| CN111072041A (en) * | 2019-12-24 | 2020-04-28 | 燕山大学 | Method for rapidly preparing two-dimensional boron alkene |
| CN115385350A (en) * | 2022-09-05 | 2022-11-25 | 深圳大学 | Preparation method and application of hydroxylated boron alkene material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402053A (en) * | 2014-11-04 | 2015-03-11 | 中国科学院大学 | Preparation method for graphene-like two-dimension nanosheet |
| CN106219608A (en) * | 2016-07-06 | 2016-12-14 | 中山大学 | A kind of preparation method of two-dimensional material |
-
2017
- 2017-05-05 CN CN201710313194.4A patent/CN107055561B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402053A (en) * | 2014-11-04 | 2015-03-11 | 中国科学院大学 | Preparation method for graphene-like two-dimension nanosheet |
| CN106219608A (en) * | 2016-07-06 | 2016-12-14 | 中山大学 | A kind of preparation method of two-dimensional material |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109149541A (en) * | 2018-09-16 | 2019-01-04 | 河南师范大学 | A kind of nanoscale demand limiter based on boron hydride alkene |
| CN109149541B (en) * | 2018-09-16 | 2019-07-26 | 河南师范大学 | A kind of nanoscale demand limiter based on boron hydride alkene |
| CN109775710A (en) * | 2019-03-16 | 2019-05-21 | 南昌大学 | A kind of preparation method of nitrogen-doped porous carbon material and the application in supercapacitor |
| CN109775710B (en) * | 2019-03-16 | 2021-05-25 | 南昌大学 | Preparation method of nitrogen-doped porous carbon material and application of nitrogen-doped porous carbon material in supercapacitor |
| CN111072041A (en) * | 2019-12-24 | 2020-04-28 | 燕山大学 | Method for rapidly preparing two-dimensional boron alkene |
| CN115385350A (en) * | 2022-09-05 | 2022-11-25 | 深圳大学 | Preparation method and application of hydroxylated boron alkene material |
| CN115385350B (en) * | 2022-09-05 | 2023-08-18 | 深圳大学 | Preparation method and application of hydroxylated boron alkene material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107055561B (en) | 2018-12-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107055561B (en) | A kind of preparation method of boron alkene | |
| Yan et al. | A quantitative method to characterize the Al4C3-formed interfacial reaction: The case study of MWCNT/Al composites | |
| CN104528703B (en) | Preparation method of nitrogen/phosphorus-codoped graphene | |
| Wu et al. | Thermodynamics and kinetics of boron removal from metallurgical grade silicon by addition of high basic potassium carbonate to calcium silicate slag | |
| Tian et al. | Analysis of magnesia carbothermic reduction process in vacuum | |
| Zhou et al. | Synthesis and ethanol-sensing properties of flowerlike SnO2 nanorods bundles by poly (ethylene glycol)-assisted hydrothermal process | |
| Jiang et al. | Fabrication of B4C from Na2B4O7+ Mg+ C by SHS method | |
| CN103922331A (en) | Method of preparing graphene powder | |
| CN113526474B (en) | Lithium nitride particles, and method and apparatus for producing same | |
| Zhang et al. | Synthesis and structural evolution of B4C–SiC nanocomposite powders by mechanochemical processing and subsequent heat treatment | |
| CN105502366A (en) | Method for preparing graphene by using biomass as raw materials | |
| Lu et al. | Rapid synthesis of single phase Gd2Zr2O7 pyrochlore waste forms by microwave sintering | |
| Wu et al. | Preparation and purification of titanium carbide via vacuum carbothermic reduction of ilmenite | |
| Wang et al. | EBSD characterization of the growth mechanism of SiC synthesized via direct microwave heating | |
| Liu et al. | Structural characterization of AlMgB14 prepared by field-activated, pressure-assisted synthesis | |
| Xiao et al. | Synthesis of nano sized Cr2AlC powders by molten salt method | |
| CN106672951A (en) | Environment-friendly, high-efficiency and large-scale graphene preparation method | |
| Bai et al. | Architecting boron nanostructure on the diamond particle surface | |
| CN104402450A (en) | Method for quickly preparing Ti2AlN ceramic powder on the basis of thermal explosion reaction at low temperature | |
| Kalvani et al. | Microstructure evolution in high density AZO ceramic sputtering target fabricated via multistep sintering | |
| Yue et al. | Study on purification of flaky graphite by argon arc plasma torch | |
| CN104495845B (en) | A kind of pure Fe3the preparation technology of C block | |
| CN104961138A (en) | Preparation method of <10>B-enriched zirconium diboride powder | |
| Chen et al. | The preparation and composition design of boron-rich lanthanum hexaboride target for sputtering | |
| Jiang et al. | Experimental study on carbothermic reduction of magnesia with different carbon materials |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |