CN103787288A - Method for preparing boron nitride alkene nanosheet - Google Patents
Method for preparing boron nitride alkene nanosheet Download PDFInfo
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- CN103787288A CN103787288A CN201410029564.8A CN201410029564A CN103787288A CN 103787288 A CN103787288 A CN 103787288A CN 201410029564 A CN201410029564 A CN 201410029564A CN 103787288 A CN103787288 A CN 103787288A
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Abstract
The invention discloses a method for preparing a boron nitride alkene nanosheet. The boron nitride alkene nanosheet takes sodium borohydride as a boron source, ammonium sulfate as a nitrogen source and a graphene nanosheet as a template. The method comprises the following steps: (1) respectively weighing ammonium sulfate, sodium borohydride and the graphene nanosheet according to a mass ratio of (1.5-1.67):1:(0.13-0.33); (2) uniformly mixing the three raw materials, putting the mixture into a reaction kettle, sealing the reaction kettle, putting into a crucible furnace for heating to be at 500-600 DEG C, preserving the temperature for 10-16 hours, and stopping heating to cool to be at room temperature along with the furnace; (3) washing an obtained product for 3-5 hours by using hydrochloric acid, subsequently washing for 3-5 times by using deionzed water, and performing suction filtration till the filtrate is neutral; (4) drying an obtained product for 5-8 hours in a drying box at 60-90 DEG C; (5) subsequently heating the dried product to be at 700-800 DEG C in a muffle furnace so as to obtain offwhite boron nitride alkene nanosheet. The equipment used in the method is simple and good in security, low in cost, stable in preparation process, simple in operation treatment and high in production efficiency.
Description
Technical field
The present invention relates to a kind of machine non-metallic material preparation method for material, especially a kind of boron nitride alkene nanometer sheet preparation method.
Background technology
From 2004, the people such as Novoselov and Geim successfully prepared the Graphene that only has one deck carbon atom, had successfully opened thus the prelude of the research of two-dimensional material.H-BN has similar structure to graphite, and the individual layer boron nitride nanosheet therefore equally with two-dirnentional structure also more and more receives investigator's concern.
Similar to Graphene, individual layer boron nitride nanosheet (boron nitride alkene) also has excellent physical properties, good mechanical property, high chemical stability and oxidation-resistance, thermal conductivity approximately 2000 W/ (m K), high-clarity (visible region is substantially without absorbing).In addition, its band gap width has reached 5.97eV.Research for individual layer boron nitride nanometer piece performance is at the early-stage, and a lot of performances are also tested.
Boron nitride alkene nanometer sheet is to be formed by individual layer boron nitride alkene two dimensional structure stacking, two dimension nano materials that thickness is nanoscale.
At present, the method for preparing boron nitride alkene nanometer sheet comprises: mechanically peel method, ultrasonic secondary solvent stripping method, chemical Vapor deposition process, SiC epitaxial growth method etc.Boron nitride alkene nanometer sheet defect prepared by mechanically peel method (for example ball milled) is many, and boron nitride alkene nanometer sheet output prepared by additive method is very little, and the transfer process complexity of boron nitride alkene nanometer sheet.
Summary of the invention
The object of the invention is, for overcoming above-mentioned the deficiencies in the prior art, provides a kind of preparation method of boron nitride alkene nanometer sheet, and the method is not used catalyzer, and cost is lower, and manipulation is simple, and raw amount is high, good product performance.
For achieving the above object, the present invention adopts following technical proposals:
A preparation method for boron nitride alkene nanometer sheet, its take sodium borohydride as boron source, ammonium sulfate is as nitrogenous source, graphene nanometer sheet are as template, concrete steps are as follows:
(1) take respectively ammonium sulfate, sodium borohydride and graphene nanometer sheet; Wherein, ammonium sulfate, sodium borohydride and graphene nanometer sheet are 1.5 ~ 1.67:1:0.13 ~ 0.33 in mass ratio;
(2) three kinds of raw materials in step (1) are mixed and packed in reactor, be tamping reactor, put in crucible oven and be heated to 500 ~ 600 ° of C, insulation 10 ~ 16 h, stop heating and make it cool to room temperature with the furnace;
(3) by hydrochloric acid cleaning 3 ~ 5 times of step (2) reaction products therefrom, then use washed with de-ionized water 3 ~ 5 times, suction filtration is until filtrate is neutrality;
(4) step (3) products therefrom is dried in loft drier to 5 ~ 8 h at 60 ~ 90 ° of C;
(5) then dried product in step (4) is heated to 700 ~ 800 ° of C oxide treatment in muffle furnace, obtains linen boron nitride alkene nanometer sheet.
Described step (1) is adopted and is weighed with scale.
The thickness of described graphene nanometer sheet is 1 ~ 20 nm.
Concentration of hydrochloric acid in described step (3) is 37.5%.
The linen boron nitride alkene of gained nanometer sheet obtains finished product through grinding, and carries out other sign and test.
Beneficial effect of the present invention is:
(1) equipment that the present invention uses is simple.The present invention uses stainless steel autoclave, is tube furnace, to requirement for experiment condition harshness and chemical gas-phase reaction method and SiC epitaxial growth method are used.Need higher vacuum tightness, generally use hazardous gas ammonia.
(2) cost is lower, and desired raw material is all conventional industrial chemicals.The raw material using in the present invention as ammonium sulfate, sodium borohydride be all common reagent.And chemical gas-phase reaction method need to use tinsel, SiC epitaxial growth method is used SiC wafer etc., and price is more expensive.
(3) stable preparation process, manipulation is simple, and production efficiency is high.Adopt the amount of boron nitride alkene nanometer sheet prepared by mechanically peel method and ultrasonic solvent stripping method considerably less, and the magnitude that the nanometer sheet of one time to produce of the present invention can reach at most gram.In addition, boron nitride alkene nanometer sheet prepared by chemical gas-phase reaction method and SiC epitaxial growth method all needs to shift, and this process operation is complicated and quality product is had to infringement.
(4) excellent product performance.Boron nitride alkene nanometer sheet and the graphene nanometer sheet prepared by the method have similar excellent properties, can be used as matrix material wild phase, sensor, semiconductor diode, field emission device etc.
Accompanying drawing explanation
Fig. 1 is the x-ray diffraction pattern of the boron nitride alkene nanometer sheet of embodiment 1;
Fig. 2 is the scanning electron microscope shape appearance figure of the boron nitride alkene nanometer sheet of embodiment 1;
Fig. 3 is the transmission electron microscope shape appearance figure of the boron nitride alkene nanometer sheet of embodiment 1;
Fig. 4 is the high-resolution electron microscopy shape appearance figure of the boron nitride alkene nanometer sheet of embodiment 1;
Fig. 5 is the SEM shape appearance figure of the boron nitride alkene nanometer sheet of embodiment 2;
Fig. 6 is the SEM shape appearance figure of the boron nitride alkene nanometer sheet of embodiment 3;
Fig. 7 is the HRTEM figure of the boron nitride alkene nanometer sheet of embodiment 4;
Fig. 8 is the SEM shape appearance figure of the boron nitride alkene nanometer sheet of embodiment 5;
Fig. 9 is the HRTEM figure of the boron nitride alkene nanometer sheet of embodiment 6.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further described.
Embodiment 1:
In order to sodium borohydride be boron source, take ammonium sulfate as nitrogenous source, graphene nanometer sheet prepares boron nitride alkene nanometer sheet as template.Weigh in the balance and get 1.5g sodium borohydride, 2.4g ammonium sulfate and 0.2g graphene nanometer sheet, pack in reactor, is tamping reactor, puts in crucible oven and be heated to 600 ° of C, and insulation 12 h, stop heating and make it cool to room temperature with the furnace; To react products therefrom hydrochloric acid cleaning 3 times, and then use washed with de-ionized water 3 times, suction filtration is until filtrate is neutrality; Then it is dried in loft drier to 6 h at 80 ° of C; Dried product is heated to 750 ° of C in muffle furnace and carries out oxide treatment, obtain linen boron nitride alkene nanometer sheet.Through grinding, obtain finished product.
Fig. 1 uses 1.5g sodium borohydride, and 2.4g ammonium sulfate and 0.2g graphene nanometer sheet are heated to 600 ° of C, insulation 12 h, and 750 ° of C oxide treatment obtain the x-ray diffraction pattern of canescence boron nitride alkene nanometer sheet.Diffraction peak in figure is all characteristic diffraction peaks of h-BN, and diffraction peak is obvious, there is no other materials that detects other, illustrates that product purity after treatment is high, well-crystallized.
Fig. 2 uses 1.5g sodium borohydride, and 2.4g ammonium sulfate and 0.2g graphene nanometer sheet are heated to 600 ° of C, insulation 12 h, and 750 ° of C oxide treatment obtain the SEM shape appearance figure of linen boron nitride alkene nanometer sheet.Can find out that boron nitride alkene nanometer sheet is energy printing opacity, shows the very thin thickness of boron nitride alkene nanometer sheet.And the area of boron nitride alkene nanometer sheet has reached micron order.
Fig. 3 and Fig. 4 use 1.5g sodium borohydride, and 2.4g ammonium sulfate and 0.2g graphene nanometer sheet are heated to 600 ° of C, insulation 12 h, and 750 ° of C oxide treatment obtain TEM shape appearance figure and the HRTEM figure of linen boron nitride alkene nanometer sheet.As can be seen from the figure, the thinner thickness of boron nitride alkene nanometer sheet, thickness is about 5nm.
Embodiment 2:
In order to sodium borohydride be boron source, take ammonium sulfate as nitrogenous source, graphene nanometer sheet prepares boron nitride nanosheet as template.Weigh in the balance and get 1.5g sodium borohydride, 2.45g ammonium sulfate and 0.3g graphene nanometer sheet, pack in reactor, is tamping reactor, puts in crucible oven and be heated to 550 ° of C, and insulation 15 h, stop heating and make it cool to room temperature with the furnace; To react products therefrom hydrochloric acid cleaning 3 times, and then use washed with de-ionized water 5 times, suction filtration is until filtrate is neutrality; Then it is dried in loft drier to 5.5 h at 70 ° of C; Dried product is heated to 730 ° of C in muffle furnace and carries out oxide treatment, obtain linen boron nitride alkene nanometer sheet.Through grinding, obtain finished product.
Fig. 5 uses 1.5g sodium borohydride, and 2.45g ammonium sulfate and 0.3g graphene nanometer sheet are heated to 550 ° of C, insulation 15 h, and 730 ° of C oxide treatment obtain the SEM shape appearance figure of linen boron nitride alkene nanometer sheet.The amount that can find out boron nitride alkene nanometer sheet is larger, but has certain curling.
Embodiment 3:
In order to sodium borohydride be boron source, take ammonium sulfate as nitrogenous source, graphene nanometer sheet prepares boron nitride nanosheet as template.Weigh in the balance and get 1.45g sodium borohydride, 2.5g ammonium sulfate and 0.4g graphene nanometer sheet, pack in reactor, is tamping reactor, puts in crucible oven and be heated to 580 ° of C, and insulation 14 h, stop heating and make it cool to room temperature with the furnace; To react products therefrom hydrochloric acid cleaning 3 times, and then use washed with de-ionized water 4 times, suction filtration is until filtrate is neutrality; Then it is dried in loft drier to 8 h at 65 ° of C; Dried product is heated to 770 ° of C in muffle furnace and carries out oxide treatment, obtain linen boron nitride alkene nanometer sheet.Through grinding, obtain finished product.
Fig. 6 uses 1.45g sodium borohydride, and 2.5g ammonium sulfate and 0.4g graphene nanometer sheet are heated to 580 ° of C, insulation 8 h, and 770 ° of C oxide treatment obtain the SEM shape appearance figure of linen boron nitride alkene nanometer sheet.The area that can find out boron nitride alkene nanometer sheet has also reached micron order, but boron nitride alkene nanometer sheet also exists some particles around, and this may be due to slightly short causing of soaking time.
Embodiment 4:
In order to sodium borohydride be boron source, take ammonium sulfate as nitrogenous source, graphene nanometer sheet prepares boron nitride nanosheet as template.Weigh in the balance and get 1.55g sodium borohydride, 2.46g ammonium sulfate and 0.3g graphene nanometer sheet, pack in reactor, is tamping reactor, puts in crucible oven and be heated to 520 ° of C, and insulation 16 h, stop heating and make it cool to room temperature with the furnace; To react products therefrom hydrochloric acid cleaning 3 times, and then use washed with de-ionized water 4 times, suction filtration is until filtrate is neutrality; Then it is dried in loft drier to 7.5 h at 75 ° of C; Dried product is heated to 720 ° of C in muffle furnace and carries out oxide treatment, obtain linen boron nitride alkene nanometer sheet.Through grinding, obtain finished product.
Fig. 7 uses 1.55g sodium borohydride, and 2.46g ammonium sulfate and 0.3g graphene nanometer sheet are heated to 520 ° of C, insulation 16 h, and 720 ° of C oxide treatment obtain the HRTEM figure of linen boron nitride alkene nanometer sheet.As can be seen from the figure, also have some unformed BN particles near boron nitride alkene nanometer sheet, this is because temperature of reaction is lower slightly.
Embodiment 5: in order to sodium borohydride be boron source, take ammonium sulfate as nitrogenous source, graphene nanometer sheet prepares boron nitride alkene nanometer sheet as template.Weigh in the balance and get 1.5g sodium borohydride, 2.25g ammonium sulfate and 0.2g graphene nanometer sheet, pack in reactor, is tamping reactor, puts in crucible oven and be heated to 500 ° of C, and insulation 10 h, stop heating and make it cool to room temperature with the furnace; To react products therefrom hydrochloric acid cleaning 3 times, and then use washed with de-ionized water 3 times, suction filtration is until filtrate is neutrality; Then it is dried in loft drier to 5 h at 60 ° of C; Dried product is heated to 700 ° of C in muffle furnace and carries out oxide treatment, obtain linen boron nitride alkene nanometer sheet.Through grinding, obtain finished product.
Fig. 8 uses 1.5g sodium borohydride, and 2.25g ammonium sulfate and 0.2g graphene nanometer sheet are heated to 500 ° of C, insulation 10h, and 700 ° of C oxide treatment obtain the HRTEM figure of linen boron nitride alkene nanometer sheet.As can be seen from the figure, boron nitride alkene nanometer sheet pattern is poor, and thickness is also larger.This is because ammonium sulfate addition is less, reacts required nitrogenous source deficiency, and in addition, temperature of reaction is also lower slightly.
Embodiment 6:
In order to sodium borohydride be boron source, take ammonium sulfate as nitrogenous source, graphene nanometer sheet prepares boron nitride alkene nanometer sheet as template.Weigh in the balance and get 1.5g sodium borohydride, 2.55g ammonium sulfate and 0.5g graphene nanometer sheet, pack in reactor, is tamping reactor, puts in crucible oven and be heated to 600 ° of C, and insulation 16 h, stop heating and make it cool to room temperature with the furnace; To react products therefrom hydrochloric acid cleaning 5 times, and then use washed with de-ionized water 5 times, suction filtration is until filtrate is neutrality; Then it is dried in loft drier to 8 h at 90 ° of C; Dried product is heated to 800 ° of C in muffle furnace and carries out oxide treatment, obtain linen boron nitride alkene nanometer sheet.Through grinding, obtain finished product.
Fig. 9 uses 1.5g sodium borohydride, and 2.55g ammonium sulfate and 0.5g graphene nanometer sheet are heated to 600 ° of C, insulation 16 h, and 800 ° of C oxide treatment obtain the HRTEM figure of linen boron nitride alkene nanometer sheet.As can be seen from the figure, boron nitride alkene nanometer sheet has reached micron order, but the fold on surface is slightly many.
By reference to the accompanying drawings the specific embodiment of the present invention is described although above-mentioned; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various modifications that creative work can make or distortion still in protection scope of the present invention.
Claims (5)
1. a preparation method for boron nitride alkene nanometer sheet, is characterized in that, its take sodium borohydride as boron source, ammonium sulfate is as nitrogenous source, graphene nanometer sheet are as template, concrete steps are as follows:
(1) take respectively ammonium sulfate, sodium borohydride and graphene nanometer sheet; Wherein, ammonium sulfate, sodium borohydride and graphene nanometer sheet are 1.5 ~ 1.67:1:0.13 ~ 0.33 in mass ratio;
(2) three kinds of raw materials in step (1) are mixed and packed in reactor, be tamping reactor, put in crucible oven and be heated to 500 ~ 600 ° of C, insulation 10 ~ 16 h, stop heating and make it cool to room temperature with the furnace;
(3) by hydrochloric acid cleaning 3 ~ 5 times of step (2) reaction products therefrom, then use washed with de-ionized water 3 ~ 5 times, suction filtration is until filtrate is neutrality;
(4) step (3) products therefrom is dried in loft drier to 5 ~ 8 h at 60 ~ 90 ° of C;
(5) then dried product in step (4) is heated to 700 ~ 800 ° of C oxide treatment in muffle furnace, obtains linen boron nitride alkene nanometer sheet.
2. the preparation method of boron nitride alkene nanometer sheet as claimed in claim 1, is characterized in that, described step (1) is adopted and weighed with scale.
3. the preparation method of boron nitride alkene nanometer sheet as claimed in claim 1, is characterized in that, the thickness of described graphene nanometer sheet is 1 ~ 20 nm.
4. the preparation method of boron nitride alkene nanometer sheet as claimed in claim 1, is characterized in that, the concentration of hydrochloric acid in described step (3) is 37.5%.
5. the preparation method of boron nitride alkene nanometer sheet as claimed in claim 1, is characterized in that, the linen boron nitride alkene of gained nanometer sheet obtains finished product through grinding.
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| CN104637898A (en) * | 2014-12-08 | 2015-05-20 | 上海大学 | Thermally conductive composite layer of integrated circuit device and electronic device thermal conduction structure packaging method |
| CN105293453A (en) * | 2015-11-20 | 2016-02-03 | 汕头大学 | Doped hexagonal boron nitride nano sheet, preparation method thereof, catalyst using same as carrier, and applications thereof |
| CN108328585A (en) * | 2018-05-03 | 2018-07-27 | 河北工业大学 | A kind of preparation method of boron nitride coated graphite alkene nanometer sheet |
| CN110655048A (en) * | 2019-11-09 | 2020-01-07 | 徐少晨 | Preparation method of silicon nitride nanosheet |
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| CN104637898A (en) * | 2014-12-08 | 2015-05-20 | 上海大学 | Thermally conductive composite layer of integrated circuit device and electronic device thermal conduction structure packaging method |
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| CN105293453A (en) * | 2015-11-20 | 2016-02-03 | 汕头大学 | Doped hexagonal boron nitride nano sheet, preparation method thereof, catalyst using same as carrier, and applications thereof |
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| CN111433156A (en) * | 2018-02-07 | 2020-07-17 | 国立大学法人东京工业大学 | Boron atomic layer sheet, laminated sheet, method for producing same, and liquid crystal |
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| CN108328585A (en) * | 2018-05-03 | 2018-07-27 | 河北工业大学 | A kind of preparation method of boron nitride coated graphite alkene nanometer sheet |
| CN110655048A (en) * | 2019-11-09 | 2020-01-07 | 徐少晨 | Preparation method of silicon nitride nanosheet |
| CN112294840A (en) * | 2020-11-02 | 2021-02-02 | 深圳北京大学香港科技大学医学中心 | Two-dimensional nanomaterial vascular plaque scavenger, M2 type macrophage inducer and autophagy modulator |
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| CN112745132A (en) * | 2020-12-24 | 2021-05-04 | 徐州康纳高新材料科技有限公司 | High-compactness high-strength quartz ceramic matrix composite material and preparation method thereof |
| CN114293050A (en) * | 2021-12-13 | 2022-04-08 | 南京航空航天大学 | Two-dimensional boron-alkene reinforced metal matrix composite material and preparation method thereof |
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Inventor after: Bi Zhenyu Inventor after: Chen Yafei Inventor after: Pei Bihong Inventor after: Bi Jianqiang Inventor after: Yin Chonglong Inventor after: You Guanglei Inventor after: Bai Yujun Inventor after: Zhao Qingqiang Inventor before: Bi Jianqiang Inventor before: Chen Yafei Inventor before: Yin Chonglong Inventor before: You Guanglei Inventor before: Bai Yujun Inventor before: Zhao Qingqiang |
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