In situ preparation method for novel iron/carbon nano-tube grading nano-composite material

Abstract

The invention relates to a preparation method for a novel iron / carbon nano-tube grading nano-composite material. The method comprises the following concrete steps: adopting ceramic arks to respectively load a precursor of iron and an organic compound of carbon source; placing the ceramic arks in a tube furnace, heating to a temperature of 300-450 DEG C under the protection of inert gas, and holding the temperature for 30 minutes; continuously heating to the temperature of 450-900 DEG C, and holding the temperature for 1-4 hours; after completing the reaction, cooling to the room temperature along with the furnace under the protection of inert gas to obtain the novel iron / carbon nano-tube grading nano-composite material. According to the present invention, the preparation process is simple, and the forming mechanism is unique; the addition of any templates, any surfactants or any structural guideline agents during the reaction process is not required; the method has characteristics of low cost and high efficiency, and is easy to industrially apply and popularize; the prepared novel iron / carbon nano-tube grading nano-composite material has strong magnetic responsibility; the morphology and the composition of the iron / carbon nano-tubes can be controlled by the reaction temperature, the reaction time and the feed ratio.

Description

technical field

[0001] The invention relates to the field of nanocomposite technology, in particular to a simple method for in-situ preparation of novel iron / carbon nanotube hierarchical nanocomposite materials. Background technique

[0002] In recent years, complex three-dimensional nanostructured materials constructed from simple building blocks (such as nanoparticles, nanorods / tubes, nanosheets, etc.) have attracted extensive attention. This is because complex nanostructures not only maintain the basic properties of the original building blocks, but also bring some new physical and chemical properties. Among them, multi-morphic carbon-based magnetic composite materials are favored in the fields of electromagnetic shielding and absorbing materials, rechargeable batteries, chemical catalytic materials, optoelectronic materials, and magnetic recording materials. On the one hand, it has the advantages of abundant raw materials, cheap price, and non-toxicity; on the other han...

Examples

Embodiment 1

[0041] Load 1 milliliter of iron pentacarbonyl and 2 grams of polyethylene glycol 20000 in ceramic arks of 8 cm × 1.2 cm × 1 cm respectively, place them in a tube furnace (inner diameter × tube length = Φ2 cm × 60 cm), and raise the temperature under nitrogen protection After heat preservation at 300°C for 30 minutes, continue to raise the temperature to 700°C and heat preservation for 2 hours. After the reaction was completed, it was cooled to room temperature with the furnace under the protection of nitrogen, and the morphology of the resulting product was as follows: figure 1 and figure 2 Shown is a new iron / carbon nanotube hierarchical nanocomposite. image 3 The EDS spectrum of the product shows that the mass percentages of carbon and iron are 75.60% and 24.40%, respectively. The TEM image of the product was observed under the transmission electron microscope Figure 4 , it can be seen that the carbon on the surface of the hierarchical structure exists in the form of ...

Embodiment 2

[0043] The process in Example 1 was adopted, except that when the iron pentacarbonyl was 2 ml and the shielding gas was a mixed gas of nitrogen and argon (volume ratio=1:1). The morphology of the obtained product is as Figure 5 and Figure 6 Shown is a new iron / carbon nanotube hierarchical nanocomposite. Figure 7 The EDS spectrum of the product shows that the mass percentages of carbon and iron are 66.17% and 33.83%, respectively. This indicates that adjusting the mass ratio of organic matter to iron source can not only change the morphology of the product, but also regulate the composition of the product.

Embodiment 3

[0045] Adopt the technique in embodiment 2, difference is: when polyethylene glycol 20000 is 0.5 gram. From Figure 8 The EDS spectrum of the elemental composition analysis shows that the mass percentages of carbon and iron are 10.88% and 89.12% respectively. The morphology of the obtained product is as Figure 9 and Figure 10 shown. Because the relative content of organic matter is small, the carbon source is low and the carbon tubes grown on the surface are short. This indicates that adjusting the relative content of carbon source can also adjust the morphology of the product.

technical field

[0001] The invention relates to the field of nanocomposite technology, in particular to a simple method for in-situ preparation of novel iron / carbon nanotube hierarchical nanocomposite materials. Background technique

[0002] In recent years, complex three-dimensional nanostructured materials constructed from simple building blocks (such as nanoparticles, nanorods / tubes, nanosheets, etc.) have attracted extensive attention. This is because complex nanostructures not only maintain the basic properties of the original building blocks, but also bring some new physical and chemical properties. Among them, multi-morphic carbon-based magnetic composite materials are favored in the fields of electromagnetic shielding and absorbing materials, rechargeable batteries, chemical catalytic materials, optoelectronic materials, and magnetic recording materials. On the one hand, it has the advantages of abundant raw materials, cheap price, and non-toxicity; on the other han...

Examples

Embodiment 1

[0041] Load 1 milliliter of iron pentacarbonyl and 2 grams of polyethylene glycol 20000 in ceramic arks of 8 cm × 1.2 cm × 1 cm respectively, place them in a tube furnace (inner diameter × tube length = Φ2 cm × 60 cm), and raise the temperature under nitrogen protection After heat preservation at 300°C for 30 minutes, continue to raise the temperature to 700°C and heat preservation for 2 hours. After the reaction was completed, it was cooled to room temperature with the furnace under the protection of nitrogen, and the morphology of the resulting product was as follows: figure 1 and figure 2 Shown is a new iron / carbon nanotube hierarchical nanocomposite. image 3 The EDS spectrum of the product shows that the mass percentages of carbon and iron are 75.60% and 24.40%, respectively. The TEM image of the product was observed under the transmission electron microscope Figure 4 , it can be seen that the carbon on the surface of the hierarchical structure exists in the form of ...

Embodiment 2

[0043] The process in Example 1 was adopted, except that when the iron pentacarbonyl was 2 ml and the shielding gas was a mixed gas of nitrogen and argon (volume ratio=1:1). The morphology of the obtained product is as Figure 5 and Figure 6 Shown is a new iron / carbon nanotube hierarchical nanocomposite. Figure 7 The EDS spectrum of the product shows that the mass percentages of carbon and iron are 66.17% and 33.83%, respectively. This indicates that adjusting the mass ratio of organic matter to iron source can not only change the morphology of the product, but also regulate the composition of the product.

Embodiment 3

[0045] Adopt the technique in embodiment 2, difference is: when polyethylene glycol 20000 is 0.5 gram. From Figure 8 The EDS spectrum of the elemental composition analysis shows that the mass percentages of carbon and iron are 10.88% and 89.12% respectively. The morphology of the obtained product is as Figure 9 and Figure 10 shown. Because the relative content of organic matter is small, the carbon source is low and the carbon tubes grown on the surface are short. This indicates that adjusting the relative content of carbon source can also adjust the morphology of the product.

Images