Preparation method of nano-hydroxyapatite/nano-hydroxyapatite gas sensing material

A nano-hydroxyapatite and gas sensing technology, which is applied in the field of nano-gas sensing materials and gas sensing, can solve the problems of long reaction time, long reaction cycle, high equipment and energy costs, etc.

Active Publication Date: 2014-07-30
CENT SOUTH UNIV
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  • Abstract
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Problems solved by technology

However, this method needs to be carried out at higher temperature, and the microstructure inside the composite is difficult to control
Gururaj M et al. used ethylenediamine to reduce graphene oxide to obtain graphene precursor, and obtained graphene / hydroxyapatite composite material by co-precipitation method (J. Materials Research Bulletin.(2010).08.077). This method uses When it comes to the toxic reagent ethylenediamine, the mass production process will pollute the environment
Chinese patents CN201210055981.0 and CN201310296678.4 use graphene oxide as a precursor, and use hydrothermal method to reduce graphene oxide to prepare nano-hydroxyapatite at the same time, thereby obtaining graphene / HA composite. The equipment and energy of this method The cost is high and the reaction time is long, which makes little sense for mass production
Hongyan Liu et al. used dopamine to reduce and modify graphene oxide, and then synthesized graphene / hydroxyapatite composite material by biomineralization (J.Phys.Chem.C2012, 116, 3334-3341). The hydroxyphosphorus obtained by this method Limestone is nano-spherical, but its crystallinity is poor. Because the reaction is carried out in simulated body fluid, the reaction period is long, and the amount of HA loaded on the graphene sheet is very small.

Method used

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[0035] This embodiment is based on the preparation method of the gas sensor of nano-hydroxyapatite / graphene gas sensing material (refer to figure 1 ), including the following steps.

[0036] a. 0.02 g of graphene oxide was ultrasonically treated at 60 kHz for 2 h to form a well-dispersed monolithic graphene oxide suspension of 1 mg / ml. Dissolve 0.04 mg of dopamine hydrochloride in Tris-HCl solution (10 mM, pH=8.5) at a concentration of 2 mg / ml, and stir for 10 s. Then the two solutions were quickly mixed in equal volumes, magnetically stirred for 11 h, centrifuged at 12,000 rpm for 10 min, washed three times with water and twice with ethanol, and the obtained precipitate was vacuum-dried at 60°C for 12 h to obtain a powder.

[0037] b. Accurately weigh 10 mg of the hydroxylated modified graphene obtained in step a, and 60 kHz ultrasonic dispersion in pre-prepared 0.05mol / L Ca(NO 3 ) 2 4H 2 In the O solution, the concentration of graphene was controlled at 1 mg / ml, and then...

Embodiment 2

[0046] The method steps and parameters of this embodiment are basically the same as those of Embodiment 1, except that the added reducing and modifying agent is norepinephrine. The properties of the nano-hydroxyapatite / graphene gas sensing material prepared by the method steps and parameters are basically the same as those in Example 1.

Embodiment 3

[0048] The method step and parameter of present embodiment and embodiment 1 are basically the same, and difference is the Ca(OH) that calcium solution is 0.01mol / L 2 Suspension, and the phosphorus solution added dropwise is 0.006mol / L H 3 PO 4 solution. The properties of the nano-hydroxyapatite / graphene gas sensing material prepared by the method steps and parameters are basically the same as those in Example 1.

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Abstract

The invention relates to a preparation method of a nano-hydroxyapatite / nano-hydroxyapatite gas sensing material. The preparation method comprises the following steps: first, preparing a graphene oxide dispersion liquid by an ultrasonic method; preparing hydroxylated modified graphene through reduction and modification of a mussel foot fibronectin analogue; in-situ reducing nucleation and growth of nucleation by a chemical precipitation method; and centrifugalizing, washing and drying to obtain the nano-hydroxyapatite / nano-hydroxyapatite gas sensing material. A gas sensor element can be prepared by the following steps: preparing the obtained gas sensing material with a binder to slurry; coating the slurry on a base body with an electrode; and then, sintering and welding for 3 hours at 300 DEG C under a nitrogen protective atmosphere.

Description

technical field [0001] The invention relates to the field of nanometer gas sensing material and gas sensing technology, in particular to a preparation method of nanometer hydroxyapatite / graphene gas sensing material and its application in gas sensor. Background technique [0002] Nanomaterials have the characteristics of large specific surface area, superior electrical and adsorption properties, etc., and have been greatly developed in the field of gas sensing. As a special two-dimensional nanomaterial, graphene has a very high active surface and electrical conductivity, and has a high signal-to-noise ratio in the detection of gas sensing performance, which has attracted more and more attention. Theoretically, the response of graphene to gas can reach the molecular level, but in practical application, in the process of graphene's response to gas, the resistance often fails to return to the original level, and positive or negative drift occurs. At present, researchers genera...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B25/32G01N27/12C01B32/194
Inventor 刘咏张青谭彦妮李会霞冯萍罗兰兰郑治
Owner CENT SOUTH UNIV
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