CN102874773B - Preparation method of porous nickel selenide hollow nanospheres - Google Patents
Preparation method of porous nickel selenide hollow nanospheres Download PDFInfo
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- CN102874773B CN102874773B CN201210330587.3A CN201210330587A CN102874773B CN 102874773 B CN102874773 B CN 102874773B CN 201210330587 A CN201210330587 A CN 201210330587A CN 102874773 B CN102874773 B CN 102874773B
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Abstract
The invention belongs to the technical field of nanometer material, relates to a synthetic method for preparing porous hollow nanospheres with uniform appearance through a hydrothermal process, and particularly relates to a preparation method of porous nickel selenide hollow nanospheres. The preparation method comprises the steps as follows: positioning selenium dioxide and nickel nitrate into alkaline aqueous solution of ammonia water; and preparing the porous hollow nanospheres through the hydrothermal process under the reduction effect of hydrazine hydrate. The nickel selenide hollow nanospheres prepared by the preparation method provided by the invention have the diameter of 300 to 400nm, and are formed by self-assembling 30 to 50nm of porous nickel selenide. The preparation method provided by the invention is simple in technology, and high in repeatability; and the used nickel source and selenium source are the inorganic compounds, low in cost, easy to obtain, low in cost, and meets the environment-friendly requirement; the method can be conducted without pre-processing such as ageing and roasting; the resultant temperature is low, therefore, the energy consumption and the reacting cost are reduced; and the mass production can be conveniently conducted.
Description
Technical field
The invention belongs to nano material preparing technical field, relate to the synthetic method of utilizing hydrothermal method to prepare the porous nano hollow ball of pattern homogeneous, particularly a kind of preparation method of porous nickelous selenide nano-hollow ball.
Background technology
The band gap of selenide semiconductor material is generally between 0.3 to 3.0 eV, it is a kind of important direct band gap N-type semiconductorN material, there is good semiconductor property, have boundless application prospect at aspects such as light emitting semiconductor device, photoelectric device, thermounits.For their research of the character such as preparation method and optical, electrical, magnetic, oneself becomes the focus that current people pay close attention to.Thereby in the last few years, a large amount of research had been carried out in preparation method, performance and the application of people to selenide semiconductor nano material, and had obtained certain achievement.Chinese patent CN100526216C discloses a kind of preparation method of Nano nickelous diselenide in hexagon, this invention is taking oleic acid as tensio-active agent, taking selenium powder as selenium source, taking organic solvent as reaction medium, adopt chemical solution method to prepare the Nano nickelous diselenide of the well-regulated hexagonal configuration of tool.First nickel salt, selenium source and tensio-active agent are mixed in organic solvent, preparation feedback liquid, then carries out solvent heat treatment by the reaction solution preparing, and controls temperature and reaction times, can obtain the Nano nickelous diselenide in hexagon of pattern rule.But the method with an organic solvent participates in reaction, and environment is had to certain influence, and synthetic be two nickelous selenide nano materials.
Nickelous selenide is a kind of important IV-VI family semi-conductor, and as a kind of rich content, environmental friendliness and chemically stable semiconductor material, nickelous selenide itself is again a kind of magneticsubstance, is a kind of following storage medium that has very much potential using value.So searching technique simply, the preparation method of the nickelous selenide nano material of multiform looks is very necessary cheaply, studies on this basis the magnetic property of nickelous selenide material, for becoming following novel storage medium, it provides scientific basis and technical support.
Summary of the invention
The object of the present invention is to provide the preparation method of the porous nickelous selenide nano-hollow ball that a kind of technique is simple, synthesis temperature is lower.
The preparation method of porous nickelous selenide nano-hollow ball, is the alkaline aqueous solution that tin anhydride and nickelous nitrate is placed in to ammoniacal liquor, under the reductive action of hydrazine hydrate, is prepared from through hydrothermal method.
A preparation method for porous nickelous selenide nano-hollow ball is to carry out according to following step:
Steps A, by tin anhydride, nickelous nitrate and deionized water short mix and stir, obtain transparent clear liquor, it is tin anhydride that wherein said each material applies ratio: nickelous nitrate: deionized water is 1 ~ 2mmol:1 ~ 2 mmol:16 ~ 20mL;
Step B, add 8 ~ 12mL strong aqua, stir it is mixed, wherein said strong aqua concentration is 25% ~ 28%;
Step C, add 8 ~ 12mL hydrazine hydrate again, stir and it is mixed, the concentration of wherein said hydrazine hydrate is 85%;
Step D, above-mentioned mixed system is transferred in teflon-lined reactor, constant temperature 2h at 140 ~ 180 DEG C of temperature, naturally cooling, obtains hydrothermal product;
Step e, by hydrothermal product centrifugation described in step D, wash respectively three times with dehydrated alcohol and deionized water;
Step F, by the product after the centrifugation of step e institute at 60 ~ 80 DEG C of vacuum-drying 6 ~ 12h, can obtain porous nickelous selenide nano-hollow ball.
The present invention adopts liquid phase method under low temperature to prepare the porous nickelous selenide nano-hollow ball of the relative homogeneous of pattern through hydro-thermal reaction.
Nickelous selenide in the present invention (NiSe) structure is determined by x-ray diffractometer, in x-ray diffraction pattern, there is no the peak of other material, this collection of illustrative plates shows, is pure nickelous selenide (NiSe) by the prepared nickelous selenide of hydrothermal method (NiSe).
Field emission scanning electron microscope (SEM) test shows, at room temperature, is about 30 ~ 50nm, the nanometer ball of 300 ~ 400nm that self-assembly forms by the prepared nickelous selenide of hydrothermal method (NiSe) by granular size; It is hollow that transmission electron microscope (TEM) demonstrates prepared nickelous selenide nanometer ball; Graph of pore diameter distribution in nitrogen adsorption-desorption (BET) test shows that the surface of its nanometer ball presents the structure of porous.
The magnetic performance test of nickelous selenide in the present invention (NiSe) porous nano hollow ball adopts vibrating sample magnetometer (VSM), and at room temperature, field intensity is from-5KOe to 5KOe.
Nickelous selenide (NiSe) the porous nano hollow ball of being prepared by liquid phase method and self-assembling technique combined technology in wood invention, on the synthetic basis of success, carry out the research of magnetic property, find that its coercive force is at room temperature 180Oe, saturation magnetization is 0.142emu/g; In magnetic, being also to have larger coercive force, is a kind of novel magnetic and stored material that has very much development potentiality.
beneficial effect
Adopt combine with the self-assembling technique nickelous selenide (NiSe) of preparation of simple liquid phase reaction, pattern is porous nano hollow structure, and this material has the advantages such as chemical stability is better.Technique of the present invention is simple, favorable reproducibility, and nickel used source, selenium source be mineral compound, and cheap and easy to get, cost is low, meets environmental friendliness requirement, due to present method do not need ageing, calcining and so on pre-treatment, synthesis temperature is lower, thereby has reduced energy consumption and reaction cost, is convenient to batch production.
Brief description of the drawings
The X-ray diffraction analysis figure (XRD) of Fig. 1 porous nickelous selenide nano-hollow ball.
The scanning electron microscope (SEM) photograph (SEM) of Fig. 2 porous nickelous selenide nano-hollow ball.
The transmission electron microscope picture (TEM) of Fig. 3 porous nickelous selenide nano-hollow ball.
The adsorption-desorption collection of illustrative plates of Fig. 4 porous nickelous selenide nano-hollow ball (insertion be graph of pore diameter distribution).
Fig. 5 porous nickelous selenide nano-hollow ball magnetic hysteresis loop at room temperature.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail, so that those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
embodiment 1
The preparation of porous nickelous selenide nano-hollow ball, comprises the steps:
Steps A, by tin anhydride, nickelous nitrate and deionized water according to tin anhydride: nickelous nitrate: the ratio of deionized water is 1mmol:1mmol:18mL ratio short mix and stirs, obtains transparent clear liquor;
Step B, add 10mL strong aqua (25% ~ 28%), stir and it is mixed;
Step C, add 12mL hydrazine hydrate (85%) again, stir and it is mixed;
Step D, mixed system is transferred in teflon-lined reactor, constant temperature 2h at 180 DEG C of temperature, naturally cooling, obtains hydrothermal product;
Step e, by hydrothermal product centrifugation described in step D, wash respectively three times with dehydrated alcohol and deionized water;
Step F, by the product after the centrifugation of step e institute at 80 DEG C of vacuum-drying 12h, can obtain porous nickelous selenide nano-hollow ball.
The XRD figure spectrum of the porous nano hollow ball of nickelous selenide (NiSe) is shown in accompanying drawing 1, and product morphology analysis is shown in accompanying drawing 2～accompanying drawing 4, and the magnetic hysteresis loop under room temperature is shown in accompanying drawing 5.
In accompanying drawing 1 position of each diffraction peak and relative intensity all with JCPDS(JCPDS) card (02-0892) matches, and in XRD figure spectrum, there is no other diffraction peak of mix, illustrate that the thing of the nickelous selenide of being prepared by liquid phase-self-assembly method (NiSe) of the present invention's proposition is pure mutually under hydrothermal condition.
In accompanying drawing 2, field emission scanning electron microscope (SEM) test shows, at room temperature, is about 30 ~ 50nm, the nanometer ball of the 300 ~ 400nm being self-assembled into by the prepared nickelous selenide of hydrothermal method (NiSe) by granular size.
In accompanying drawing 3, it is hollow that transmission electron microscope (TEM) demonstrates prepared nickelous selenide nanometer ball.
In accompanying drawing 4, the graph of pore diameter distribution in nitrogen adsorption-desorption (BET) test shows that the surface of its nanometer ball presents the structure of porous, and the diameter in duct mostly is 3.8nm.
In accompanying drawing 5, can find that nickelous selenide (NiSe) coercive force is at room temperature 180Oe, saturation magnetization is 0.142emu/g; In magnetic, being also to have larger coercive force, is a kind of novel magnetic and stored material that has very much development potentiality.
embodiment 2
The preparation of porous nickelous selenide nano-hollow ball, comprises the steps:
Steps A, by tin anhydride, nickelous nitrate and deionized water according to tin anhydride: nickelous nitrate: the ratio of deionized water is 1mmol:1mmol:20mL ratio short mix and stirs, obtains transparent clear liquor;
Step B, add 8mL strong aqua (25% ~ 28%), stir and it is mixed;
Step C, add 12mL hydrazine hydrate (85%) again, stir and it is mixed;
Step D, mixed system is transferred in teflon-lined reactor, constant temperature 2h at 140 DEG C of temperature, naturally cooling, obtains hydrothermal product;
Step e, by hydrothermal product centrifugation described in step D, wash respectively three times with dehydrated alcohol and deionized water;
Step F, by the product after the centrifugation of step e institute at 60 DEG C of vacuum-drying 12h, can obtain porous nickelous selenide nano-hollow ball.
embodiment 3
The preparation of porous nickelous selenide nano-hollow ball, comprises the steps:
Steps A, by tin anhydride, nickelous nitrate and deionized water according to tin anhydride: nickelous nitrate: the ratio of deionized water is 1mmol:2mmol:20mL ratio short mix and stirs, obtains transparent clear liquor;
Step B, add 10mL strong aqua (25% ~ 28%), stir and it is mixed;
Step C, add 10mL hydrazine hydrate (85%) again, stir and it is mixed;
Step D, mixed system is transferred in teflon-lined reactor, constant temperature 2h at 180 DEG C of temperature, naturally cooling, obtains hydrothermal product;
Step e, by hydrothermal product centrifugation described in step D, wash respectively three times with dehydrated alcohol and deionized water;
Step F, by the product after the centrifugation of step e institute at 80 DEG C of vacuum-drying 12h, can obtain porous nickelous selenide nano-hollow ball.
embodiment 4
The preparation of porous nickelous selenide nano-hollow ball, comprises the steps:
Steps A, by tin anhydride, nickelous nitrate and deionized water according to tin anhydride: nickelous nitrate: the ratio of deionized water is 2mmol:1mmol:16mL ratio short mix and stirs, obtains transparent clear liquor;
Step B, add 12mL strong aqua (25% ~ 28%), stir and it is mixed;
Step C, add 12mL hydrazine hydrate (85%) again, stir and it is mixed;
Step D, mixed system is transferred in teflon-lined reactor, constant temperature 2h at 140 DEG C of temperature, naturally cooling, obtains hydrothermal product;
Step e, by hydrothermal product centrifugation described in step D, wash respectively three times with dehydrated alcohol and deionized water;
Step F, by the product after the centrifugation of step e institute at 60 DEG C of vacuum-drying 6h, can obtain porous nickelous selenide nano-hollow ball.
embodiment 5
The preparation of porous nickelous selenide nano-hollow ball, comprises the steps:
Steps A, by tin anhydride, nickelous nitrate and deionized water according to tin anhydride: nickelous nitrate: the ratio of deionized water is 2mmol:1.5mmol:16mL ratio short mix and stirs, obtains transparent clear liquor;
Step B, add 12mL strong aqua (25% ~ 28%), stir and it is mixed;
Step C, add 12mL hydrazine hydrate (85%) again, stir and it is mixed;
Step D, mixed system is transferred in teflon-lined reactor, constant temperature 2h at 180 DEG C of temperature, naturally cooling, obtains hydrothermal product;
Step e, by hydrothermal product centrifugation described in step D, wash respectively three times with dehydrated alcohol and deionized water;
Step F, by the product after the centrifugation of step e institute at 80 DEG C of vacuum-drying 12h, can obtain porous nickelous selenide nano-hollow ball.
embodiment 6
The preparation of porous nickelous selenide nano-hollow ball, comprises the steps:
Steps A, by tin anhydride, nickelous nitrate and deionized water according to tin anhydride: nickelous nitrate: the ratio of deionized water is 1mmol:1.5mmol:18mL ratio short mix and stirs, obtains transparent clear liquor;
Step B, add 10mL strong aqua (25% ~ 28%), stir and it is mixed;
Step C, add 12mL hydrazine hydrate (85%) again, stir and it is mixed;
Step D, mixed system is transferred in teflon-lined reactor, constant temperature 2h at 180 DEG C of temperature, naturally cooling, obtains hydrothermal product;
Step e, by hydrothermal product centrifugation described in step D, wash respectively three times with dehydrated alcohol and deionized water;
Step F, by the product after the centrifugation of step e institute at 70 DEG C of vacuum-drying 12h, can obtain porous nickelous selenide nano-hollow ball.
embodiment 7
The preparation of porous nickelous selenide nano-hollow ball, comprises the steps:
Steps A, by tin anhydride, nickelous nitrate and deionized water according to tin anhydride: nickelous nitrate: the ratio of deionized water is 1mmol:1mmol:20mL ratio short mix and stirs, obtains transparent clear liquor;
Step B, add 12mL strong aqua (25% ~ 28%), stir and it is mixed;
Step C, add 8mL hydrazine hydrate (85%) again, stir and it is mixed;
Step D, mixed system is transferred in teflon-lined reactor, constant temperature 2h at 140 DEG C of temperature, naturally cooling, obtains hydrothermal product;
Step e, by hydrothermal product centrifugation described in step D, wash respectively three times with dehydrated alcohol and deionized water;
Step F, by the product after the centrifugation of step e institute at 60 DEG C of vacuum-drying 12h, can obtain porous nickelous selenide nano-hollow ball.
Claims (1)
1. a preparation method for porous nickelous selenide nano-hollow ball, is characterized in that carrying out according to following step:
Steps A, by tin anhydride, nickelous nitrate and deionized water short mix and stir, obtain transparent clear liquor, it is tin anhydride that wherein said each material applies ratio: nickelous nitrate: deionized water is 1 ~ 2mmol:1 ~ 2 mmol:16 ~ 20mL;
Step B, add 8 ~ 12mL strong aqua, stir it is mixed, wherein said strong aqua concentration is 25% ~ 28%;
Step C, add 8 ~ 12mL hydrazine hydrate again, stir and it is mixed, the concentration of wherein said hydrazine hydrate is 85%;
Step D, above-mentioned mixed system is transferred in teflon-lined reactor, constant temperature 2h at 140 ~ 180 DEG C of temperature, naturally cooling, obtains hydrothermal product;
Step e, by hydrothermal product centrifugation described in step D, wash respectively three times with dehydrated alcohol and deionized water;
Step F, by the product after the centrifugation of step e institute at 60 ~ 80 DEG C of vacuum-drying 6 ~ 12h, can obtain porous nickelous selenide nano-hollow ball.
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| CN103755548B (en) * | 2013-12-30 | 2015-08-19 | 上海交通大学 | Hydrazine hydrate hydrothermal conversion CO 2for the method for formic acid |
| CN103985813B (en) * | 2014-06-04 | 2016-08-17 | 北京科技大学 | Nucleocapsid structure NiSe2@SiO2composite thermoelectric material and preparation method |
| CN105016314B (en) * | 2015-02-05 | 2017-02-22 | 天津大学 | Preparation method for zinc selenide nano hollow spheres |
| CN106024395B (en) * | 2016-07-01 | 2018-07-06 | 淮阴工学院 | A kind of Ni based on nickel foam3Se2The preparation method and applications of nano material |
| CN106744728B (en) * | 2016-12-19 | 2019-03-05 | 陕西科技大学 | A kind of method that room temperature liquid phase method prepares SnSe micron ball |
| CN108493297B (en) * | 2018-03-23 | 2020-03-10 | 福州大学 | Preparation method of three-dimensional hollow selenium nickel sulfide nano-frame catalyst |
| CN108878153B (en) * | 2018-06-28 | 2019-09-13 | 福州大学 | A kind of ferrous selenide nickel dye-sensitized solar cells is to electrode |
| CN108899207A (en) * | 2018-06-28 | 2018-11-27 | 福州大学 | One-step method growth in situ nickelous selenide solar battery is to electrode and its preparation method and application |
| CN108840313B (en) * | 2018-09-19 | 2022-07-08 | 曲阜师范大学 | Preparation method of multistage spherical nickel diselenide |
| CN110950311B (en) * | 2019-12-13 | 2021-04-23 | 西南大学 | Preparation method of nickel selenide micro-nano flower, product and application thereof |
| KR102477409B1 (en) * | 2020-12-21 | 2022-12-15 | 동국대학교 산학협력단 | Air electrode for Lithium Air Battery and Method of manufacturing the same |
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| CN101049917A (en) * | 2007-03-29 | 2007-10-10 | 上海交通大学 | Method for preparing Nano nickelous diselenide in hexagon |
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