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Preparation method of batch preparation of boron nitride nanotube

A boron nitride nanotube, batch technology, applied in chemical instruments and methods, nitrogen compounds, nanotechnology and other directions, can solve the problems that restrict the wide application of boron nitride nanotubes, high preparation temperature, complex process, etc., and achieve a wide range of industrial applications. The effect of application value, simple preparation process and wide source of raw materials

Inactive Publication Date: 2013-01-02
JINGDEZHEN CERAMIC INSTITUTE
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Problems solved by technology

[0003] The commonly used preparation methods of boron nitride nanotubes include arc discharge method, laser ablation method, template method, mechanical ball milling method, CVD and thermal decomposition method, etc., but these methods have low yield, low purity, high preparation temperature and high cost. Or the disadvantages of complex process and difficult industrialization, the obtained boron nitride nanotubes have many defects in different shapes, which seriously restricts the wide application of boron nitride nanotubes

Method used

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  • Preparation method of batch preparation of boron nitride nanotube
  • Preparation method of batch preparation of boron nitride nanotube

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Effect test

Embodiment 1

[0022] 称取5克无定形B粉,1.45克Fe 2 o 3 ,1.27克CaO,充分混合后平铺在氧化铝瓷板上,置于管式炉内,充入氩气保护并开始升温,氩气流量为300ml / min,升温至1000℃时,停止通入氩气,开始通入NH 3 , NH 3 流量为150ml / min,并继续加热至1300℃,保温4个小时,保温结束后停止通入任何气体,关闭管式炉进、出气口,自然降温至室温,得到白色粗产物,将粗产物在空气中加热至600℃进行氧化处理,将氧化后的粗产物放入浓度为38wt%的盐酸中浸泡6小时,抽滤,洗涤,干燥后可得到9.9克BN纳米管粉体,以B粉为基准计算其产率为87%,BN纳米管的纯度约为90%,所制备出的氮化硼纳米管为多壁纳米管,平均管径为150nm,长度大于100微米,管身均匀光滑。

Embodiment 2

[0024] 称取7克B 2 o 3 ,0.42克Co 2 o 3 ,0.78克BaO,充分混合后平铺在氧化铝瓷板上,置于管式炉内,充入氩气保护并开始升温,氩气流量为300ml / min,升温至1100℃时,停止通入氩气,开始通入NH 3 , NH 3 流量为200ml / min,并继续加热至1400℃,保温3个小时,保温结束后停止通入任何气体,关闭管式炉进、出气口,自然降温至室温,得到白色粗产物,将粗产物在空气中加热至600℃进行氧化处理,将氧化后的粗产物放入浓度为36wt%的盐酸中浸泡12小时,抽滤,洗涤,干燥后可得到4.3克BN纳米管粉体,以B 2 o 3 粉为基准计算其产率为85%,BN纳米管的纯度约为85%,所制备出的氮化硼纳米管为多壁纳米管,平均管径为180nm,长度大于100微米,管身均匀 smooth.

Embodiment 3

[0026] 称取6.2克H 3 BO 3 ,0.4克Fe 2 o 3 ,1.48克Ca(OH) 2 ,充分混合后平铺在氧化铝瓷板上,置于管式炉内,充入氩气保护并开始升温,氩气流量为500ml / min,升温至1000℃时,停止通入氩气,开始通入NH 3 , NH 3 流量为300ml / min,并继续加热至1200℃,保温4个小时,保温结束后停止通入任何气体,关闭管式炉进、出气口,自然降温至室温,得到白色粗产物,将粗产物在空气中加热至600℃进行氧化处理,将氧化后的粗产物放入浓度为37wt%的盐酸中浸泡8小时,抽滤,洗涤,干燥后可得到2.2克BN纳米管粉体,以H 3 BO 3 粉为基准计算其产率为88%,BN纳米管的纯度约为85%,所制备出的氮化硼纳米管为多壁纳米管,平均管径为120nm,长度大于100微米,管身均匀 smooth.

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Abstract

The invention relates to a method for batch preparation of boron nitride nanotubes. The method comprises the steps of sufficiently mixing a boron source, a transition metal compound and alkaline-earth metal compounds; heating the mixture to 1000-1100 DEG C under the protection of nitrogen or argon; stopping supplying a protective gas, beginning supplying a mixture gas of the nitrogen and the argon, reacting and continuing to heat to 1200-1400 DEG C, keeping the temperature for 0.5-4 hours, stopping the supply of the gas after the heat preservation, closing the gas inlet and the gas outlet and decreasing the temperature to the room temperature so as to obtain white rough products, heating the rough products in the air to 600 DEG C and subsequently pickling and drying. The diameter of the prepared boron nitride nanotube is 50-300nm, and the length can be more than 100 microns. By introducing an alkaline-earth metal as a catalyst, a great quantity of boron nitride nanotubes can grow at a lower temperature; the cost is lower, the material resource is wide, the preparation process is simple, and the batch production can be realized easily.

Description

technical field [0001] 本发明属于无机纳米材料领域,具体涉及一种批量制备氮化硼纳米管的制备方法。 Background technique [0002] 氮化硼纳米管类似于碳纳米管,可以看做是碳纳米管中的碳原子被硼和氮原子交替取代的产物。 氮化硼纳米管不仅具有可以与碳纳米管相媲美的力学性能和热传导性能,而且还具有优异的抗氧化性、化学稳定性和热稳定性,这使得氮化硼纳米管成为理想的在结构材料,应用于纳米复合材料中。 氮化硼纳米管为稳定的宽带隙材料,电学性能不随管径和手性改变,这相对于碳纳米管易变的电学性能而言,氮化硼纳米管在电子器件中的应用具有较大 The advantages. 此外,氮化硼纳米管还具有较好的储氢性能,阴极射线发射性能和生物相容性,这些优点可使氮化硼纳米管在能源,场致发光和生物医用领域具有潜在的应用价值。 [0003] 常用的氮化硼纳米管制备方法有电弧放电法,激光烧蚀法,模板法,机械球磨法,CVD以及热分解法等,但这些方法存在产率低,纯度低,制备温度高,成本高或者工艺复杂难以产业化等缺点,所得到的氮化硼纳米管形态各异缺陷也较多,这严重制约着氮化硼纳米管的广泛应用。 Contents of the invention [0004] 本发明的目的在于解决现有技术中的问题,提供一种产率高、纯度高、制备条件温和、成本低、工艺简单的氮化硼纳米管的制备方法,而且该制备方法易于放大,可以达到批量生产的目的。 [0005] 本发明的技术方案是:一种批量制备氮化硼纳米管的方法,其特征在于:将硼源,过渡金属化合物以及碱土金属化合物充分混合,将混合物在氮气或氩气保护下加热至1000~1100℃,停止通入保护气体,开始通入氨气或者氮气与氢气的混合气体进行反应并继续加热至1200~1400℃,保温0.5~4小时,保温结束后停止气体的通入并将温度降至室温,得到白色粗产物,将粗产物在空气中加热至600℃后,经酸洗、干燥获得管径为50~300nm、长度可达100微米以上的氮化硼纳米管。 [0006] 所述混合物包含的硼源中硼元素、过渡金属、碱土金属的摩尔比为1:0.01~0.09:0.03~0.27。 [0007] 所述的硼源为硼粉或氧化硼或硼酸。 [0008] 所述的过渡金属化合物为Fe或Co或Ni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/064B82Y30/00
Inventor 刘维良班晓磊冯震乾曾小军
Owner JINGDEZHEN CERAMIC INSTITUTE
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