CN102874773A - Preparation method of porous nickel selenide hollow nanospheres - Google Patents
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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 the 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, have good semiconductor property, at aspects such as light emitting semiconductor device, photoelectric device, thermounits boundless application prospect is arranged.For their research of preparation method and the character such as light, electricity, magnetic, oneself becomes the focus that present people pay close attention to.Thereby in the last few years, people had carried out a large amount of research to selenide semiconductor preparations of nanomaterials method, performance and application, and had obtained certain achievement.Chinese patent CN100526216C discloses a kind of preparation method of Nano nickelous diselenide in hexagon, this invention is take oleic acid as tensio-active agent, take selenium powder as selenium source, take organic solvent as reaction medium, adopt chemical solution method to prepare the Nano nickelous diselenide of the well-regulated hexagonal configuration of tool.At first nickel salt, selenium source and tensio-active agent are mixed in the organic solvent, then preparation feedback liquid carry out solvent heat treatment with the reaction solution for 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 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 potential using value is arranged very much.So searching technique simply, the nickelous selenide preparations of nanomaterials method 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 ammoniacal liquor, under the reductive action of hydrazine hydrate, is prepared from through hydrothermal method.
A kind of preparation method of porous nickelous selenide nano-hollow ball is to carry out according to following step:
Steps A, with 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, adding 8 ~ 12mL strong aqua, stirring mixes it, and 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 the teflon-lined reactor, constant temperature 2h under 140 ~ 180 ℃ of temperature, naturally cooling obtains hydrothermal product;
Step e, with the described hydrothermal product centrifugation of step D, wash respectively three times with dehydrated alcohol and deionized water;
Step F, with the product after the centrifugation of step e institute at 60 ~ 80 ℃ of vacuum-drying 6 ~ 12h, can obtain porous nickelous selenide nano-hollow ball.
The present invention adopts liquid phase method under the low temperature to prepare the porous nickelous selenide nano-hollow ball of the relative homogeneous of pattern through hydro-thermal reaction.
Nickelous selenide among the present invention (NiSe) structure is determined do not have the peak of other material to exist in the x-ray diffraction pattern by x-ray diffractometer, 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 by the prepared nickelous selenide of hydrothermal method (NiSe) by granular size, the nanometer ball of 300 ~ 400nm that self-assembly forms; 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.
Vibrating sample magnetometer (VSM) is adopted in the test of the magnetic performance of nickelous selenide among the present invention (NiSe) porous nano hollow ball, and at room temperature, field intensity is from-5KOe to 5KOe.
Nickelous selenide (NiSe) the porous nano hollow ball that is prepared by liquid phase method and self-assembling technique combined technology in the wood invention, carry out the research of magnetic property on the basis that success is synthetic, find that its coercive force at room temperature is 180Oe, saturation magnetization is 0.142emu/g; Also being to have larger coercive force on magnetic, is a kind of novel magnetic and stored material that development potentiality is arranged very much.
Beneficial effect
Adopt combine with the self-assembling technique nickelous selenide (NiSe) of preparation of simple liquid phase reaction, pattern is the 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 used nickel source, selenium source be mineral compound, and cheap and easy to get, cost is low, meets the environmental friendliness requirement, because present method does not need the pre-treatment of ageing, calcining and so on, synthesis temperature is lower, thereby has reduced energy consumption and reaction cost, is convenient to batch production.
Description of 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
The present invention is described in detail below in conjunction with embodiment, so that those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
The preparation of porous nickelous selenide nano-hollow ball comprises the steps:
Steps A, with 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 the teflon-lined reactor, constant temperature 2h under 180 ℃ of temperature, naturally cooling obtains hydrothermal product;
Step e, with the described hydrothermal product centrifugation of step D, wash respectively three times with dehydrated alcohol and deionized water;
Step F, with the product after the centrifugation of step e institute at 80 ℃ 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 seen accompanying drawing 1, and the product morphology analysis is seen accompanying drawing 2～accompanying drawing 4, and the magnetic hysteresis loop under the room temperature is seen accompanying drawing 5.
In the accompanying drawing 1 position of each diffraction peak and relative intensity all with JCPDS(JCPDS) card (02-0892) matches, and do not have other diffraction peak of mix in the XRD figure spectrum, illustrate that the phase of the nickelous selenide (NiSe) of being prepared by liquid phase-self-assembly method of the present invention's proposition is pure under hydrothermal condition.
In accompanying drawing 2, field emission scanning electron microscope (SEM) test shows, at room temperature, is about 30 ~ 50nm by the prepared nickelous selenide of hydrothermal method (NiSe) by granular size, the nanometer ball of the 300 ~ 400nm that is self-assembled into.
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 at room temperature is 180Oe, saturation magnetization is 0.142emu/g; Also being to have larger coercive force on magnetic, is a kind of novel magnetic and stored material that development potentiality is arranged very much.
The preparation of porous nickelous selenide nano-hollow ball comprises the steps:
Steps A, with 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 the teflon-lined reactor, constant temperature 2h under 140 ℃ of temperature, naturally cooling obtains hydrothermal product;
Step e, with the described hydrothermal product centrifugation of step D, wash respectively three times with dehydrated alcohol and deionized water;
Step F, with the product after the centrifugation of step e institute at 60 ℃ of vacuum-drying 12h, can obtain porous nickelous selenide nano-hollow ball.
The preparation of porous nickelous selenide nano-hollow ball comprises the steps:
Steps A, with 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 the teflon-lined reactor, constant temperature 2h under 180 ℃ of temperature, naturally cooling obtains hydrothermal product;
Step e, with the described hydrothermal product centrifugation of step D, wash respectively three times with dehydrated alcohol and deionized water;
Step F, with the product after the centrifugation of step e institute at 80 ℃ of vacuum-drying 12h, can obtain porous nickelous selenide nano-hollow ball.
The preparation of porous nickelous selenide nano-hollow ball comprises the steps:
Steps A, with 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 the teflon-lined reactor, constant temperature 2h under 140 ℃ of temperature, naturally cooling obtains hydrothermal product;
Step e, with the described hydrothermal product centrifugation of step D, wash respectively three times with dehydrated alcohol and deionized water;
Step F, with the product after the centrifugation of step e institute at 60 ℃ of vacuum-drying 6h, can obtain porous nickelous selenide nano-hollow ball.
The preparation of porous nickelous selenide nano-hollow ball comprises the steps:
Steps A, with 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 the teflon-lined reactor, constant temperature 2h under 180 ℃ of temperature, naturally cooling obtains hydrothermal product;
Step e, with the described hydrothermal product centrifugation of step D, wash respectively three times with dehydrated alcohol and deionized water;
Step F, with the product after the centrifugation of step e institute at 80 ℃ 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, with 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 the teflon-lined reactor, constant temperature 2h under 180 ℃ of temperature, naturally cooling obtains hydrothermal product;
Step e, with the described hydrothermal product centrifugation of step D, wash respectively three times with dehydrated alcohol and deionized water;
Step F, with the product after the centrifugation of step e institute at 70 ℃ 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, with 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 the teflon-lined reactor, constant temperature 2h under 140 ℃ of temperature, naturally cooling obtains hydrothermal product;
Step e, with the described hydrothermal product centrifugation of step D, wash respectively three times with dehydrated alcohol and deionized water;
Step F, with the product after the centrifugation of step e institute at 60 ℃ of vacuum-drying 12h, can obtain porous nickelous selenide nano-hollow ball.
Claims (2)
1. the preparation method of a porous nickelous selenide nano-hollow ball is characterized in that carrying out according to following step:
Steps A, with 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, adding 8 ~ 12mL strong aqua, stirring mixes it, and 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 the teflon-lined reactor, constant temperature 2h under 140 ~ 180 ℃ of temperature, naturally cooling obtains hydrothermal product;
Step e, with the described hydrothermal product centrifugation of step D, wash respectively three times with dehydrated alcohol and deionized water;
Step F, with the product after the centrifugation of step e institute at 60 ~ 80 ℃ of vacuum-drying 6 ~ 12h, can obtain porous nickelous selenide nano-hollow ball.
2. the porous nickelous selenide nano-hollow ball of described method preparation according to claim 1 is characterized in that the diameter of described nickelous selenide nano-hollow ball is 300 ~ 400nm, is that the nickelous selenide particle self-assembly by 30 ~ 50nm forms.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103755548A (en) * | 2013-12-30 | 2014-04-30 | 上海交通大学 | Method for hydrothermally converting CO2 into formic acid by hydrazine hydrate |
| CN103985813A (en) * | 2014-06-04 | 2014-08-13 | 北京科技大学 | NiSe2@SiO2 composite thermoelectric material with core-shell structure and preparation method thereof |
| CN105016314A (en) * | 2015-02-05 | 2015-11-04 | 天津大学 | Preparation method for zinc selenide nano hollow spheres |
| CN106024395A (en) * | 2016-07-01 | 2016-10-12 | 淮阴工学院 | Preparation method and application of foamed nickel-based Ni3Se2 nano material |
| CN106744728A (en) * | 2016-12-19 | 2017-05-31 | 陕西科技大学 | A kind of method that room temperature liquid phase method prepares SnSe micron balls |
| CN108493297A (en) * | 2018-03-23 | 2018-09-04 | 福州大学 | A kind of preparation method of three-dimensional hollow selenium nanometer nickel sulfide frame catalyst |
| CN108840313A (en) * | 2018-09-19 | 2018-11-20 | 曲阜师范大学 | A kind of preparation method of spherical two nickelous selenide of multistage |
| CN108878153A (en) * | 2018-06-28 | 2018-11-23 | 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 |
| CN110950311A (en) * | 2019-12-13 | 2020-04-03 | 西南大学 | Preparation method of nickel selenide micro-nano flower, product and application thereof |
| KR20220090596A (en) * | 2020-12-21 | 2022-06-30 | 동국대학교 산학협력단 | Air electrode for Lithium Air Battery and Method of manufacturing the same |
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| CN103755548A (en) * | 2013-12-30 | 2014-04-30 | 上海交通大学 | Method for hydrothermally converting CO2 into formic acid by hydrazine hydrate |
| CN103985813A (en) * | 2014-06-04 | 2014-08-13 | 北京科技大学 | NiSe2@SiO2 composite thermoelectric material with core-shell structure and preparation method thereof |
| CN103985813B (en) * | 2014-06-04 | 2016-08-17 | 北京科技大学 | Nucleocapsid structure NiSe2@SiO2composite thermoelectric material and preparation method |
| CN105016314A (en) * | 2015-02-05 | 2015-11-04 | 天津大学 | Preparation method for zinc selenide nano hollow spheres |
| CN106024395A (en) * | 2016-07-01 | 2016-10-12 | 淮阴工学院 | Preparation method and application of foamed nickel-based Ni3Se2 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 |
| CN106744728A (en) * | 2016-12-19 | 2017-05-31 | 陕西科技大学 | A kind of method that room temperature liquid phase method prepares SnSe micron balls |
| CN108493297A (en) * | 2018-03-23 | 2018-09-04 | 福州大学 | A kind of preparation method of three-dimensional hollow selenium nanometer nickel sulfide frame catalyst |
| CN108878153A (en) * | 2018-06-28 | 2018-11-23 | 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 |
| 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 |
| CN108840313A (en) * | 2018-09-19 | 2018-11-20 | 曲阜师范大学 | A kind of preparation method of spherical two nickelous selenide of multistage |
| CN110950311A (en) * | 2019-12-13 | 2020-04-03 | 西南大学 | Preparation method of nickel selenide micro-nano flower, product and application thereof |
| KR20220090596A (en) * | 2020-12-21 | 2022-06-30 | 동국대학교 산학협력단 | Air electrode for Lithium Air Battery and Method of manufacturing the same |
| 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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