CN104803361A - Method for increasing yield of BN (boron nitride) nanotubes prepared with ball-milling and annealing method - Google Patents
Method for increasing yield of BN (boron nitride) nanotubes prepared with ball-milling and annealing method Download PDFInfo
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- CN104803361A CN104803361A CN201510117928.2A CN201510117928A CN104803361A CN 104803361 A CN104803361 A CN 104803361A CN 201510117928 A CN201510117928 A CN 201510117928A CN 104803361 A CN104803361 A CN 104803361A
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Abstract
The invention discloses a method for increasing the yield of BN (boron nitride) nanotubes prepared with a ball-milling and annealing method. The method comprises steps as follows: crystal boron oxide powder and GGr15 steel balls with the mass ratio being 20:1 are ball-milled for 40-120 h under the protection of the high-purity N2 gas and then annealed at the high temperature of 1,100-1,300 DEG C for 7-9 h under the protection of the high-purity NH3 atmosphere by the aid of a tube type atmosphere annealing furnace, and white powder products, namely, the BN nanotubes, are prepared. With the adoption of the method for increasing the yield of the BN nanotubes prepared with the ball-milling and annealing method, reaction conditions are mild, the preparation technology is simple, the obtained BN nanotubes are uniform in thickness and good in purity, the yield is high, and electron microscope analysis indicates that the products are uniform in thickness, the yield is higher than 90% and the purity is higher than 95%.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, particularly relate to a kind of method improving ball milling annealing method and prepare boron nitride nano-tube productive rate.
Background technology
Since CNT (carbon nano-tube) finds, based on hexagonal boron nitride (BN) and graphite similarity structurally, shown by Theoretical Calculation, BN nanotube is stable on energy, there is the energy gap (being about 5.5eV) of near constant, particularly energy gap not with chirality and tube layer number change and change, this constant electrical properties makes it more have practical value than carbon nanotube.Simultaneously BN nanotube has the oxidation-resistance more outstanding than carbon nanotube, and oxidation resistance temperature is up to closely
be considered to the template of alternative carbon nanotube as resistance to high temperature oxidation to prepare other novel monodimension nanometer material.In addition, BN nanotube density is little, has good thermal conductivity, insulativity and higher mechanical property.Have experiment to prove, the Young's modulus of BN nanotube, up to 1.22 ± 0.24TPa, conforms to theoretical expectation values.Based on these feature performance benefits, BN nanotube is expected to be applied in nano-structural ceramic, single electron diode, hydrogen storage material and field emission material etc.In addition, BN nanotube good biocompatibility is good bio-medical material.
The research of current BN nanotube mainly concentrates on preparation aspect, and people have attempted synthesizing BN nanotube by multiple method, as plasma arc electric discharge, CVD thermal decomposition method, chemical method of substitution, laser ablation method and mechanical attrition method etc.Although the BN nanotube preparation method of current report is a lot, its productive rate purity all needs to be improved further.
Summary of the invention
Problem to be solved by this invention provides a kind of method improving ball milling annealing method and prepare boron nitride nano-tube productive rate for above-mentioned the deficiencies in the prior art.
The present invention adopts following technical scheme:
The method that raising ball milling annealing method of the present invention prepares boron nitride nano-tube productive rate be by crystal boron oxide powder and GGr15 steel ball with the ratio of mass ratio 20: 1 in high-purity N
2ball milling 40-120h under gas shielded, then utilizes tubular type ambient anneal stove, under 1100 DEG C ~ 1300 DEG C high temperature, at high-purity N H
3anneal under atmosphere protection 7-9 hour, obtains the BN nanotube that namely white powder product is prepared.
Ball-milling Time is preferably 80h.
High-purity N H
3the flow velocity of gas is 50ml/min.
Annealing time is preferably 8h.
Positively effect of the present invention is as follows:
The reaction conditions that raising ball milling annealing method of the present invention prepares the method for boron nitride nano-tube productive rate is gentle, and preparation technology is simple, the BN nanotube even thickness of gained, productive rate is high, purity is good, and electronic microscope photos shows that product even thickness, productive rate are more than 90%, and purity is greater than 95%.
The method reaction raw materials boron oxide that raising ball milling annealing method of the present invention prepares boron nitride nano-tube productive rate is cheap, and conversion unit is conventional, and temperature of reaction is low, productive rate and purity high, technique is easy to grasp.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of boron nitride nano-tube prepared by the embodiment of the present invention 3.
Embodiment
The following examples describe in further detail of the present invention.
Embodiment 1
The method that raising ball milling annealing method of the present invention prepares boron nitride nano-tube productive rate be by crystal boron oxide powder and GGr15 steel ball with the ratio of mass ratio 20: 1 in high-purity N
2ball milling 40h under gas shielded, then utilizes tubular type ambient anneal stove, under 1100 DEG C of DEG C of high temperature, at high-purity N H
3anneal 7 hours under atmosphere protection, obtain the BN nanotube that namely white powder product is prepared.
High-purity N H
3the flow velocity of gas is 50ml/min.
Productive rate 92%, purity 95%.
Embodiment 2
The method that raising ball milling annealing method of the present invention prepares boron nitride nano-tube productive rate be by crystal boron oxide powder and GGr15 steel ball with the ratio of mass ratio 20: 1 in high-purity N
2ball milling 120h under gas shielded, then utilizes tubular type ambient anneal stove, under 1300 DEG C of high temperature, at high-purity N H
3anneal 9 hours under atmosphere protection, obtain the BN nanotube that namely white powder product is prepared.
High-purity N H
3the flow velocity of gas is 50ml/min.
Productive rate 93%, purity 96%.
Embodiment 3
The method that raising ball milling annealing method of the present invention prepares boron nitride nano-tube productive rate be by crystal boron oxide powder and GGr15 steel ball with the ratio of mass ratio 20: 1 in high-purity N
2ball milling 80h under gas shielded, then utilizes tubular type ambient anneal stove, under 1200 DEG C of high temperature, at high-purity N H
3anneal 8 hours under atmosphere protection, obtain the BN nanotube that namely white powder product is prepared.
High-purity N H
3the flow velocity of gas is 50ml/min.
Productive rate 95%, purity 98%.
As shown in Figure 1, the boron nitride nano-tube even thickness prepared of method of the present invention.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Claims (4)
1. improve the method that ball milling annealing method prepares boron nitride nano-tube productive rate, it is characterized in that: described method be by crystal boron oxide powder and GGr15 steel ball with the ratio of mass ratio 20: 1 in high-purity N
2ball milling 40-120h under gas shielded, then utilizes tubular type ambient anneal stove, under 1100 DEG C ~ 1300 DEG C high temperature, at high-purity N H
3anneal under atmosphere protection 7-9 hour, obtains the BN nanotube that namely white powder product is prepared.
2. the method improving ball milling annealing method and prepare boron nitride nano-tube productive rate as claimed in claim 1, is characterized in that: Ball-milling Time is 80h.
3. the method improving ball milling annealing method and prepare boron nitride nano-tube productive rate as claimed in claim 1, is characterized in that: high-purity N H
3the flow velocity of gas is 50ml/min.
4. the method improving ball milling annealing method and prepare boron nitride nano-tube productive rate as claimed in claim 1, is characterized in that: annealing time is 8h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510117928.2A CN104803361A (en) | 2015-03-18 | 2015-03-18 | Method for increasing yield of BN (boron nitride) nanotubes prepared with ball-milling and annealing method |
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| CN201510117928.2A CN104803361A (en) | 2015-03-18 | 2015-03-18 | Method for increasing yield of BN (boron nitride) nanotubes prepared with ball-milling and annealing method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108545708A (en) * | 2018-03-14 | 2018-09-18 | 中国人民解放军火箭军工程大学 | A kind of preparation method of the micro-nano section of jurisdiction composite construction of coralliform hexagonal boron nitride |
| CN114261949A (en) * | 2022-02-07 | 2022-04-01 | 中国人民解放军火箭军工程大学 | Small-diameter boron nitride nanotube and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103922295A (en) * | 2014-04-17 | 2014-07-16 | 河北工业大学 | Preparation method of boron nitride nano tube |
| CN103964403A (en) * | 2014-04-08 | 2014-08-06 | 南京航空航天大学 | Preparation method of three-dimensional porous hexagonal boron nitride |
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2015
- 2015-03-18 CN CN201510117928.2A patent/CN104803361A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103964403A (en) * | 2014-04-08 | 2014-08-06 | 南京航空航天大学 | Preparation method of three-dimensional porous hexagonal boron nitride |
| CN103922295A (en) * | 2014-04-17 | 2014-07-16 | 河北工业大学 | Preparation method of boron nitride nano tube |
Non-Patent Citations (1)
| Title |
|---|
| 李艳娇 等: "机械化学法制备氮化硼纳米管及纳米粒子", 《材料热处理学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108545708A (en) * | 2018-03-14 | 2018-09-18 | 中国人民解放军火箭军工程大学 | A kind of preparation method of the micro-nano section of jurisdiction composite construction of coralliform hexagonal boron nitride |
| CN108545708B (en) * | 2018-03-14 | 2021-08-24 | 中国人民解放军火箭军工程大学 | Preparation method of coralline hexagonal boron nitride micro-nano tube sheet composite structure |
| CN114261949A (en) * | 2022-02-07 | 2022-04-01 | 中国人民解放军火箭军工程大学 | Small-diameter boron nitride nanotube and preparation method thereof |
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