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Method for producing nano nickle sphere

A nano-nickel and preparation method is applied in the field of preparation of nano-nickel balls to achieve the effects of long-term stable existence, good magnetic properties and uniform product morphology.

Inactive Publication Date: 2011-02-16
NANJING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the methods of nano-nickel materials mainly contain high-temperature pyrolysis of organometallic compounds and electrochemical reduction, (Green, M.Organometallic Based Strategies for Metal Nanocrystal Synthesis.Chem.Commun.2005, 24, 3002-3011.10.Cheng, G.J.; Puntes, V.F.; Guo, T. Synthesis and Self-Assembled Ring Structures of NiNanocrystals. J. Colloid Interface Sci. 2006, 293, 430-436.11. Hou, Y.; Kondoh, H.; Ohta, T.; Gao, S. Size -Controlled Synthesis of Nickel Nanoparticles.Appl.Surf.Sci.2005, 241, 218-222.) Microwave method, chemical reduction method, etc. (Masaharu T, Masayuki H, Takeshi T.Fast Preparation ofNano-sized Nickel Particles under Microwave Irradiation without Using Catalyst Nucleation [J]. Chem. Lett., 2002, 12 (31): 1232-1233. Cordente, N.; Amiens, C.; Chaudret, B.; Respaud, M.; Senocq, F.; Casanove, M.J. Chemisorption on Nickel Nanoparticles of Various Shapes: Influence on Magnetism. J. Appl. Phys. 2003, 94, 6358-6365. Falong Jia, Lizhi Zhang, Xiaoying Shang, and Yan Yang Adv, Ater, 2008, 20, 1050-1054), However, there is no report on the use of hydrothermal method to synthesize nickel nanomaterials with good dispersion and uniformity of different sizes.

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  • Method for producing nano nickle sphere
  • Method for producing nano nickle sphere
  • Method for producing nano nickle sphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The preparation of embodiment 1 nano-nickel sphere

[0020] Weigh nickel chloride (NiCl 2 ·6H 2 O) 0.2g, PVP 0.30g, dissolved in 5ml of water, potassium hydroxide (KOH) 0.27g, sodium hypophosphite (NaH 2 PO 2 ·H 2 O) 0.5g, dissolved in 2ml, 5ml water respectively. Mix nickel chloride, PVP solution and potassium hydroxide solution, and pass nitrogen gas, then add sodium hypophosphite solution and continue nitrogen flow for 10 minutes. The mixed solution was transferred to the inner tank of the hydrothermal kettle with a volume of 15ml, and the nitrogen protection was continued, and then the hydrothermal kettle was sealed, and the reaction was carried out at a temperature of 140°C for 40 minutes. The obtained product was washed three times with water and ethanol respectively, separated magnetically, and finally dried at below 50°C to obtain 0.032 g of black powder. The XRD pattern is shown in Figure 1A , it can be attracted by a magnet (see Figure 1B ). The parti...

Embodiment 2

[0021] The preparation of embodiment 2 nano-nickel spheres (change pH value)

[0022] Weigh nickel chloride (NiCl 2 ·6H 2 O) 0.2g, PVP 0.30g, dissolved in 5ml water, potassium hydroxide (KOH) 0.18g, sodium hypophosphite (NaH 2 PO 2 ·H 2 O) 0.5g, dissolved in 2ml, 5ml water respectively. Mix nickel chloride, PVP solution and potassium hydroxide solution, and pass nitrogen gas, then add sodium hypophosphite solution and continue nitrogen flow for 10 minutes. The mixed solution was transferred to the inner tank of the hydrothermal kettle with a volume of 15ml, and the nitrogen protection was continued, and then the hydrothermal kettle was sealed, and the reaction was carried out at a temperature of 140°C for 40 minutes. The obtained product was washed three times with water and ethanol respectively, magnetically separated, and finally dried at below 50° C. to obtain 0.035 g of black powder. The particle size of the obtained product is 100-300 nanometers, the dispersion is g...

Embodiment 3

[0023] The preparation of embodiment 3 nano-nickel spheres (change pH value)

[0024] Weigh nickel chloride (NiCl 2 ·6H 2 O) 0.2g, PVP 0.30g, dissolved in 5ml water, potassium hydroxide (KOH) 0.09g, sodium hypophosphite (NaH 2 PO 2 ·H 2O) 0.5g, dissolved in 2ml, 5ml water respectively. Mix the nickel chloride solution, the PVP solution and the potassium hydroxide solution, and pass nitrogen gas, then add the sodium hypophosphite solution and continue to pass nitrogen for 10 minutes. The mixed solution was transferred to the inner tank of the hydrothermal kettle with a volume of 15ml, and the nitrogen protection was continued, and then the hydrothermal kettle was sealed, and the reaction was carried out at a temperature of 140°C for 40 minutes. The obtained product was washed three times with water and ethanol respectively, magnetically separated, and finally dried at below 50° C. to obtain 0.036 g of black powder. The particle size of the obtained product is 300-600 nano...

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Abstract

The invention relates to a method for preparing a nanometer nickel pellet with magnetic property. Nickel dichloride, polyvinylpyrrolidone, potassium hydroxide and sodium hypophosphite are dissolved in water respectively; a nickel dichloride solution and a potassium hydroxide solution are mixed, are introduced with nitrogen gas, then added with a sodium hypophosphite solution and continuously keptin a nitrogen introducing state for 10 minutes; the mixed solution is transferred to an inner tank of a hydrothermal kettle with cubage of 15 ml and is continuously introduced with nitrogen gas for protection; the hydrothermal kettle is sealed; the mixed solution reacts for 40 to 60 minutes at a temperature of between 130 and 150 DEG C; and an obtained product is washed by water and ethanol respectively, subjected to magnetic separation and is dried to obtain the nanometer nickel pellet with the magnetic property. The nanometer nickel pellet is subjected to characteristic representation through x ray diffraction (XRD), a transmission electron microscope (TEM) and a scanning electron microscope (SEM); the result shows that the particle diameters of a series of prepared nanometer nickel pellets are between 100 and 500 nanometers; and the particle diameter is relevant to reaction temperature, PH value, dosage of a reducer, reaction time and an added surfactant.

Description

technical field [0001] The invention relates to a method for preparing a series of nano-nickel balls of different sizes. Background technique [0002] In recent years, functional nanomaterials have shown great application potential in industrial and technical fields. Nanomagnetic materials have a wide range of applications in biopharmaceuticals, magnetic resonance imaging, separation and purification of biomolecules and biological processes (Momet, S.; Vasseur, S.; Grasset, F.; Duguet, E.J.Mater.Chem.2004, 14 , 2161. Weissleder, R.; Kelly, K.; Sun, E.Y.; Shtatland, T.; Josephson, L. Nat. Biotechnol.2005, 23, 1418. Gu, H.; ; Xu, B. Chem. Commun. 2006, 941). In particular, nano-nickel with good hydrogen storage performance and catalytic activity has attracted widespread attention for its application in magnetic sensors and memory chip materials. At present, the methods of nano-nickel materials mainly contain high-temperature pyrolysis of organometallic compounds and electro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/16
Inventor 姜立萍李晔朱俊杰季鹏宇
Owner NANJING UNIV
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