CN1631588A - Method for manufacturing nanometer nickel - Google Patents
Method for manufacturing nanometer nickel Download PDFInfo
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- CN1631588A CN1631588A CN 200410084286 CN200410084286A CN1631588A CN 1631588 A CN1631588 A CN 1631588A CN 200410084286 CN200410084286 CN 200410084286 CN 200410084286 A CN200410084286 A CN 200410084286A CN 1631588 A CN1631588 A CN 1631588A
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Abstract
The invention relates to a super-micro nickel particle preparation technique, belongs to radiation chemistry manufacturing nanometer material production technique field. The invention nanometer nickel production technique is adopted with radiation chemistry method for nanometer material preparation using nickel sulfate as crude material irradiated by electron beam generated by high frequency high pressure industrial electron accelerator in certain irradiating dose of 70 to 350 KGy developing radiation reaction in the solution added with hydrophilic surfacing-activator polyvinyl alcohol and oxidating free radical scavenger isopropyl alcohol so to deoxidate the nickel ion into nickel atom step by step accumulating into crystal core and control the particle size by controlling the crystal core growing speed with hydrophilic surfacing-activator finally obtain the nanometer super-micro nickel particle. The advantages of the invention are simple technique process, short production cycle, non-polluting while the obtained nanometer nickel particles is of uniform diameter and finely divided.
Description
Technical field
The present invention relates to a kind of preparation method of nickel ultramicron, belong to radiation chemistry and make the nano material technology field.
Background technology
Having a extensive future of nanometer nickel is widely used in fields such as magnetic fluid, effective catalyst, high active combustion agent, electrocondution slurry, high performance electrode material, metal and the processing of nonmetallic surface conductance coating.
The main at present physico-chemical processes such as condensation of gas method, electrolysis, High Pressure Hydrogen reducing process that adopt of nano metal preparation method.These method conditions needed need generate nano metal powder generally all than higher under low dark decay atmosphere He in the professional equipment.Use the radiation chemistry method to prepare nano material, more widely used at present method is the gamma-rays radiation method, still, does not also have electron accelerator to prepare nanometer nickel as the method for radiation source both at home and abroad.
Summary of the invention
The object of the present invention is to provide and adopt another kind of radiation source, the electron beam that promptly adopts high-frequency and high-voltage industrial electronic accelerator to produce prepares the method for nano metal nickel as radiation source.
A kind of manufacture method of nanometer nickel adopts the radiation chemistry method to prepare nano material, it is characterized in that the processing step of this method is as follows:
A) adopting nickelous sulfate is raw material, and it is dissolved in the distilled water, and nickel concentration is 0.005-0.02mol/100ml in the solution;
B) add hydrophilic surfactant active's polyvinyl alcohol then, its concentration is 0.4-1.0g/100ml;
C) add the scavenger of isopropyl alcohol again as oxidative free radical OH; Its concentration is 15-45ml/100ml;
D) the above-mentioned mixed solution for preparing is packed in the irradiation vessel, and charge into nitrogen, seal irradiation vessel then to get rid of the oxygen in the solution;
E) adopting high-frequency and high-voltage industrial electronic accelerator, is to carry out irradiation with different irradiation doses under ground that meter electron accelerator of 2.0MeV, 10mA in working range, and irradiation dose is: 70-350KGy;
F) solution behind the irradiation is used deionized water and absolute ethanol washing repeatedly, separate with magnetic separating device, repeated multiple times is to remove unreacted nickel ion and hydrophilic surfactant active's polyvinyl alcohol in the solution
G) in vacuum drying chamber, the gained sample was carried out air drying 8-12 hour then, can obtain the nano-nickel powder end of black.
Mainly utilize the radiation chemistry principle among the present invention, adopt the source of nickelous sulfate, utilize electron beam that the industrial electronic accelerator produces to be gone back ortho states hydrogen H, aqueous electron e what aqueous solution ionization produced as nickel
- AqNickel ion reaction Deng having in reproducibility particle and the solution is reduced into nickle atom with it, and nickle atom is gathered into nucleus, controls the growth rate of nucleus by the hydrophilic surfactant active, and controls the size of particle, makes particle reach nanoscale.The adding of isopropyl alcohol is the scavenger as oxidative free radical OH in addition.
The advantage of the inventive method is: at normal temperatures and pressures, need not to add any catalyst, prepare nanometer nickel with the electron beam method of radiating.This method technical process is simple, with short production cycle, pollution-free, and the nano nickle granules particle size of preparation gained is even, good dispersion.
The specific embodiment
Now specific embodiments of the invention are described in the back:
Embodiment one: the concrete processing step of present embodiment is as follows:
A. at first, take by weighing a certain amount of nickelous sulfate, it is dissolved in the distilled water, make solution concentration reach 0.015mol/100ml with FA1004 ware formula electronic balance;
B. add hydrophilic surface active agent polyvinyl alcohol PVA then, concentration is 0.8g/100ml;
C. add oxidative free radical OH free radical scavenger isopropyl alcohol IPA again, concentration is 35ml/100ml;
D. the above-mentioned solution for preparing is packed in the irradiation vessel, charge into nitrogen, then irradiation vessel is sealed to get rid of the oxygen in the solution;
E. adopting high-frequency and high-voltage industrial electronic accelerator, is to carry out irradiation with the 200-300KGy irradiation dose under ground that meter electron accelerator of 2.0MeV, 10mA in working range;
F. the solution behind the irradiation is used deionized water and absolute ethanol washing three times, separated with magnetic separation technique again, three times repeatedly, to remove unreacted nickel ion and the hydrophilic surface active agent polyvinyl alcohol PVA in the solution;
G. in vacuum drying chamber, carry out air drying 10 hours then, can obtain the nano-nickel powder end of black.
Add hydrophilic surfactant active's polyvinyl alcohol among the present invention, can carry out surface modification to particle, cover one layer of polymeric at particle surface, particle and the growth of having controlled the particle nucleation so not only can have been stablized, and has the agglomeration that particle very easily takes place for high surface energy, high chemical energy, particle because of the metallic atom particle when having prevented solution evaporation
The gained sample fits like a glove by the peak value of the characteristic peaks in the diffraction pattern with JCPDS standard powder diffraction card (Ni-04-0850) mutually through X-ray diffractometer XRD test.Thereby can determine that this black powder absolutely is nanometer nickel.
From JEM-200CX type high resolution transmission electron microscopy tem observation, visible sample particle is spherical in shape, and granular size is comparatively even.And particle diameter is distributed between the 20-50nm.
The analysis of laser particle diameter distribution instrument shows the particle size distribution range of nanometer nickel in chloroform between 30-70nm, and its main peak appears at 39.4nm and goes out, and this and TEM experimental result are consistent.
Thermal analysis experiment result by differential scanning thermal analyzer DSC shows that when the particle diameter of nickel reached nanoscale, its fusing point was 528.5 ℃, and the fusing point of common nickel is 1455 ℃.This shows that when nickel reaches nanoscale very big change takes place the performance of material.
Claims (1)
1. the manufacture method of a nanometer nickel adopts the radiation chemistry method to prepare nano material, it is characterized in that the processing step of this method is as follows:
A) adopting nickelous sulfate is raw material, and it is dissolved in the distilled water, and nickel concentration is 0.005-0.02mol/100ml in the solution;
B) add hydrophilic surfactant active's polyvinyl alcohol then, its concentration is 0.4-1.0g/100ml;
C) add the scavenger of isopropyl alcohol again as oxidative free radical OH; Its concentration is 15-45ml/100ml;
D) the above-mentioned mixed solution for preparing is packed in the irradiation vessel, and charge into nitrogen, seal irradiation vessel then to get rid of the oxygen in the solution;
E) adopting high-frequency and high-voltage industrial electronic accelerator, is to carry out irradiation with different irradiation doses under 2.0MeV, 10mA ground that meter electron accelerator in working range, and irradiation dose is: 70-350KGy;
F) solution behind the irradiation is used deionized water and absolute ethanol washing repeatedly, separate with magnetic separating device, repeated multiple times is to remove unreacted nickel ion and hydrophilic surfactant active's polyvinyl alcohol in the solution
G) in vacuum drying chamber, the gained sample was carried out air drying 8-12 hour then, can obtain the nano-nickel powder end of black.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410084286 CN1631588A (en) | 2004-11-18 | 2004-11-18 | Method for manufacturing nanometer nickel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410084286 CN1631588A (en) | 2004-11-18 | 2004-11-18 | Method for manufacturing nanometer nickel |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1631588A true CN1631588A (en) | 2005-06-29 |
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| CN 200410084286 Pending CN1631588A (en) | 2004-11-18 | 2004-11-18 | Method for manufacturing nanometer nickel |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100391663C (en) * | 2006-04-10 | 2008-06-04 | 李小毛 | Process for preparing nano nickel powder |
| CN102247856A (en) * | 2010-05-21 | 2011-11-23 | 中国石油化工股份有限公司 | Eggshell nickel-based bifunctional hydrogenation catalyst and preparation method and application thereof |
-
2004
- 2004-11-18 CN CN 200410084286 patent/CN1631588A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100391663C (en) * | 2006-04-10 | 2008-06-04 | 李小毛 | Process for preparing nano nickel powder |
| CN102247856A (en) * | 2010-05-21 | 2011-11-23 | 中国石油化工股份有限公司 | Eggshell nickel-based bifunctional hydrogenation catalyst and preparation method and application thereof |
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