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A kind of synthetic method of NIO multilevel micro-nano fiber and the product obtained therefrom

A technology of micro-nano fiber and synthesis method, which is applied in the field of synthesis of NiO multi-level micro-nano structure, can solve problems such as difficult multi-level structure, multi-level process control factors on the surface of micro-nano materials, complex high-temperature chemical reactions, etc. Achieve the effects of controllable composition, adjustable static spinning parameters, and simple process parameters

Inactive Publication Date: 2020-02-07
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, by designing a suitable precursor reaction system and heat treatment system, there are few reports on the synthesis of NiO multi-level micro-nano structures by electrospinning technology, mainly because of the complex high-temperature chemical reactions and the multi-level surface of micro-nano materials The process is controlled by many factors, and it is difficult to form a multi-level structure

Method used

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  • A kind of synthetic method of NIO multilevel micro-nano fiber and the product obtained therefrom
  • A kind of synthetic method of NIO multilevel micro-nano fiber and the product obtained therefrom
  • A kind of synthetic method of NIO multilevel micro-nano fiber and the product obtained therefrom

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1.1 Mix 0.0437 g of p-phenylenediamine, 0.0534 g of glutaric acid, 0.4802 g of nickel chloride (NiCl 2 . 6H 2O) and 0.6660 g of PVP were dissolved in a mixed solvent consisting of 4 mL of DMF and 1 mL of ethanol, and stirred until transparent to obtain a precursor spinning solution.

[0031] 1.2 The precursor fiber was obtained by electrospinning the precursor spinning solution. The spinning parameters were: positive voltage 18KV, negative voltage 0.5 KV, receiving distance 18 cm, and syringe advancing speed 0.002 mm / s.

[0032] 1.3 Place the precursor fiber in a muffle furnace, raise the temperature from room temperature to 600 °C at a rate of 1 °C / min in an air atmosphere, and keep it for 2 h. After the sample is cooled with the furnace, NiO multi-level micro-nano fibers are obtained.

[0033] The XRD result of the product is as follows figure 1 As shown, it can be seen from the figure that all the diffraction peaks are consistent with the standard XRD card (44-115...

Embodiment 2

[0035] 2.1 Add 0.0413 g of p-phenylenediamine, 0.0216 g of glutaric acid, and 0.3241 g of NiCl 2 . 6H 2 O and 0.3297g of PVP were dissolved in a mixed solvent of 4 mL of DMF and 1 mL of ethanol, and stirred until transparent to obtain a precursor spinning solution.

[0036] 2.2 The precursor fiber was obtained by electrospinning the precursor spinning solution. The spinning parameters were: positive voltage 16KV, negative voltage 0.5 KV, receiving distance 20 cm, and syringe advancing speed 0.001 mm / s.

[0037] 2.3 Place the precursor fiber in a muffle furnace, raise the temperature from room temperature to 700 °C at a rate of 2 °C / min in an air atmosphere, and keep it for 7 h. After the sample is cooled with the furnace, the NiO multi-level micro-nano fiber is obtained. The NiO multi-level micro-nano fiber is composed of NiO porous fibers and NiO nanoparticles, and NiO nanoparticles are grown in situ on the surface of the NiO porous fibers, wherein the diameter of the NiO p...

Embodiment 3

[0039] 3.1 Add 0.0447 g of p-phenylenediamine, 0.1135 g of glutaric acid, and 0.7562 g of NiCl 2 . 6H 2 O and 1.2937g of PVP were dissolved in a mixed solvent of 4 mL of DMF and 1 mL of ethanol, and stirred until transparent to obtain a precursor spinning solution.

[0040] 3.2 The precursor fiber was obtained by electrospinning the precursor spinning solution. The spinning parameters were: positive voltage 17KV, negative voltage 0.5 KV, receiving distance 19 cm, and syringe advancing speed 0.002 mm / s.

[0041] 3.3 Place the precursor fiber in a muffle furnace, raise the temperature from room temperature to 550 °C at a rate of 3 °C / min in an air atmosphere, and keep it for 3 h. After the sample is cooled with the furnace, the NiO multi-level micro-nano fiber is obtained. The NiO multilevel micro-nanofiber is composed of NiO porous fibers and NiO nanoparticles, and NiO nanoparticles are grown in situ on the surface of the NiO porous fibers, wherein the diameter of the NiO por...

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Abstract

The invention discloses a synthesis method of NiO multi-stage micro-nano fiber and a product obtained thereby. The synthesis method comprises the following steps: dissolving p-phenylenediamine, glutaric acid, nickel salt and polyvinylpyrrolidone into a mixed solvent of dimethyl formamide and ethanol and stirring until the solution is transparent to obtain a precursor spinning solution; preparing precursor fiber from the precursor spinning solution by an electrostatic spinning method and performing heat treatment on the precursor fiber to obtain the NiO multi-stage micro-nano fiber. A novel precursor reaction system is designed, the required raw materials are low in price, operation is simple and convenient, process parameters are controllable, and the product has a special microstructure,has a typical multi-stage micro-nano structure, has high repeatability and dispersibility, is suitable for industrialized production and can play an important role in the field of gas-sensitive application.

Description

technical field [0001] The invention relates to a synthesis method of NiO multilevel micro-nano structure, in particular to an electrospinning synthesis method of NiO porous fiber whose surface grows NiO nano particles in situ and the obtained product. Background technique [0002] Semiconductor gas sensitive materials mainly include SnO 2 , ZnO, WO 3 , NiO and other oxide materials, which can show good gas response performance to different types of toxic, harmful, flammable and explosive gases such as nitrogen oxides, sulfur oxides, benzene and their derivatives, and are widely used in industrial detection , food safety, environmental detection and other fields. In order to adapt to complex conditions such as high temperature, high pressure, chemical corrosion, and low concentration that are common in the current gas detection process, it is urgent to strengthen the stability, sensitivity, and selectivity of gas-sensitive materials. Therefore, the research and developmen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/08D01F1/10D01F6/44D01D1/02D01D5/00
CPCD01D1/02D01D5/003D01F1/10D01F6/44D01F9/08
Inventor 马谦李绘陈迎张进涛韩智峰车全德王俊鹏方圆杨萍
Owner UNIV OF JINAN