CN102502893A - Preparation method of NiO nanowire and magnetic field thermal treatment device - Google Patents
Preparation method of NiO nanowire and magnetic field thermal treatment device Download PDFInfo
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Abstract
The invention relates to a preparation method of a NiO nanowire. The invention further relates to a thermal treatment device, in particular to a magnetic field thermal treatment device, more particularly to a thermal treatment device for the preparation method of the NiO nanowire. According to the preparation method of the NiO nanowire, the Ni nanowire is placed into a magnetic field environment for annealing. The magnetic field thermal treatment device comprises magnetic field generating equipment and constant temperature controlling equipment. According to the method and the device, the technical problems of complex process, high cost, unavailable batch production and severe environmental pollution existing in the conventional NiO nanowire preparation method are solved.
Description
Technical field
The present invention relates to a kind of preparation method of NiO nano wire.The invention still further relates to a kind of thermal treatment unit, particularly a kind of thermomagnetic treatment device is specifically related to a kind of thermal treatment unit that is used for the preparation method of said NiO nano wire.
Background technology
Nickel oxide (NiO) nano material is the bigger P-N-type semiconductorN functional materials of a kind of energy gap; Have excellent catalytic activity, superparamagnetism, thermo-sensitive property and electric property, have very application prospects in fields such as catalyzer, battery electrode, electrochemical capacitor, electronic component, photoelectricity converting material, magneticsubstance, function ceramics, thermal sensing element and gas sensors.In recent years, the NiO of different shape is nanocrystalline to be synthesized, as: NiO nano particle, NiO flower type structure, NiO nano chain, NiO nanometer rod, NiO nanofiber, NiO nano wire and NiO nano thin-film etc.Wherein, the NiO nano wire is because of having unique one-dimentional structure size and peculiar physics-chem characteristic, thereby has very important meaning aspect theory research and the technical application.Yet; Because the complicated process of preparation of NiO nano wire, with high costs, productive rate is lower, environmental pollution is serious; Especially lower, the easy fracture of the intensity of NiO nano wire; Hinder its further development and application, made the one dimension advantageous characteristic of one dimension P-N-type semiconductorN functional materials be difficult on using, embody.Therefore, but develop and develop simple, the with low cost industrialized mass production of a kind of technology, and the preparation method of the NiO nano wire of environmental protection has very big realistic meaning.
Through being retrieved, existing literature finds; Application number is 02156897.9; Publication number is the one Chinese patent application of CN1413946A, has put down in writing " a kind of compound method of nickel oxide nano line ", wherein discloses the method that a kind of microvoid structure that utilizes alumina formwork (AAO) prepares the NiO nano wire; The preparation process of this method comprises that preparation, the configuration of nickel salt solution, the nickel salt filling of AAO micropore, inert atmosphere roasting, the alkali lye of AAO template remove the AAO template, obtain the NiO semiconductor nanowires at last.In preparation technology's flow process; The acid solution preparation of AAO template needs a plurality of steps accurately to control pore size; The alkali lye of template is removed also needs accurately temperature, pH value, time and the uniformity coefficient of control solution; Its technology is very complicated and be difficult to the mass-producing batch process, and the discharging of adding acid solution, alkali lye will cause very big influence to environment.In the process of removing template, alkali lye makes the intensity of nano wire greatly reduce to the corrosion of NiO nano wire, and the supersound process of half hour makes nano wire be fractured into short nanometer rod or nano particle.Therefore, for this complex process, with high costs, environmental pollution is serious, and the lower preparation method of NiO nano wire intensity who prepares needs further to improve and improve.
Further retrieval is found; Switzerland's periodical " Sens.Actuators B:Chem. (sensor and actuator B) " (2011; Doi:10.1016/j.snb.2011.04.028) paper (people such as author B.Liu, H.Q.Yang, H.Zhao) of a piece of writing " Synthesis and enhanced gas-sensing properties of ultralong NiO nanowires assembled with NiO nanocrystals (raising of the synthetic and air-sensitive performance of the NiO nano wire of the nanocrystalline assembling of NiO) " by name discloses the reacted nickel powder that contains of autoclave has been heat-treated the method that makes the NiO nano wire in.This method at first with nickelous chloride, sodium oxalate and terepthaloyl moietie 220 ℃ of stainless steel autoclaves of sealing insulation 12 hours, naturally cool to room temperature then, again with product spinning, cleaning, oven dry after product 400 ℃ of thermal treatments of muffle furnace 2 hours.This preparation process is complicated, and reaction needs carries out in hyperbaric environment, adds the explained hereafter cycle long (needing 24 hours ability to prepare a stove sample), is difficult to realize suitability for industrialized production.
Application number is 200910068368.0; Publication number is the one Chinese patent application of CN101525161A; Put down in writing " a kind of method for preparing nickel oxide one dimension nano material ", wherein disclose and a kind of organic complexing agent and nickel salt mixing solutions have been carried out the method that high temperature annealing prepares the NiO nano wire.Be about to be configured to solution by a certain percentage like the organic complex and the nickel salt of gelatin, chitosan, Schardinger dextrins, Xylo-Mucine, Z 150PH and so on, in this solution, carrying out substrate immersion progressively again, high temperature (about 550 ℃) annealing makes semiconductor nanowires.The organic complex that this method is used all has functional groups such as hydroxyl, carboxyl, amino, makes the NiO nano wire top layer of preparation closely coated by these organo-functional groups, is difficult to clean and remove.Simultaneously, the NiO nano wire is assembled nano particle by these functional groups just, and therefore after removing these organo-functional groups, the NiO nano wire will be split into nanocluster or nanoparticle.
Summary of the invention
First aspect purpose of the present invention is to propose a kind of preparation method of NiO nano wire, with solve existing NiO nano wire preparation method complex process, with high costs, can't quantize to produce, technical problem that environmental pollution is serious.
The present invention solves the problems of the technologies described above through following technical scheme, reaches the object of the invention.
A kind of preparation method of NiO nano wire is characterized in that, places magnetic field environment to heat-treat the Ni nano wire, to obtain said NiO nano wire.Further, said thermal treatment is anneal.
When the preparation method of the described NiO nano wire of embodiment of the present invention, preferably, may further comprise the steps:
A) the Ni nano wire is placed magnetic field environment;
B) under magnetic field environment, heat up;
C) under magnetic field environment, be incubated;
D) under magnetic field environment, carry out naturally cooling,, promptly get said NiO nano wire until room temperature.
When the preparation method of the described NiO nano wire of embodiment of the present invention; Preferably, in said step b), the magneticstrength of said magnetic field environment is 0.05T-0.52T; The temperature rise rate of said intensification is 0.5 ℃/min-50 ℃/min, and said intensification is that to be warming up to temperature of charge be 400 ℃-1500 ℃.
When the preparation method of the described NiO nano wire of embodiment of the present invention; Preferably, in said step c), the magneticstrength of said magnetic field environment is 0.05T-0.52T; Said insulation is that the maintenance temperature of charge is 400 ℃-1500 ℃, and the soaking time of said insulation is 1.5h-15h.
When the preparation method of the described NiO nano wire of embodiment of the present invention, preferably, in said step d), the magneticstrength of said magnetic field environment is 0.05T-0.52T.
When the preparation method of the described NiO nano wire of embodiment of the present invention, preferably, the preparation method of said NiO nano wire carries out under normal pressure, in the air.
When the preparation method of the described NiO nano wire of embodiment of the present invention; One preferred embodiment is; In said step b); The magneticstrength of said magnetic field environment is 0.05T-0.52T, and the temperature rise rate of said intensification is 0.5 ℃/min-50 ℃/min, and said intensification is that to be warming up to temperature of charge be 400 ℃-1500 ℃; In said step c), the magneticstrength of said magnetic field environment is 0.05T-0.52T, and said insulation is that temperature of charge is remained on the temperature of charge after heating up in the said step b), and the soaking time of said insulation is 1.5h-15h; In said step d), the magneticstrength of said magnetic field environment is 0.05T-0.52T; The preparation method of said NiO nano wire carries out under normal pressure, in the air.
Second aspect purpose of the present invention is to propose a kind of thermomagnetic treatment device; Said thermomagnetic treatment device is applicable to the preparation method of NiO nano wire of the present invention; Use said thermomagnetic treatment device; Can prepare the NiO nano wire, solve existing NiO nano wire preparation method complex process, with high costs, can't quantize to produce, technical problem that environmental pollution is serious.
The present invention solves the problems of the technologies described above through following technical scheme, reaches the object of the invention.
A kind of thermomagnetic treatment device that is used for the preparation method of NiO nano wire comprises:
The material platform, said material platform is used for ccontaining material;
Magnetic field generating apparatus, said magnetic field generating apparatus are used for producing and regulating and control the needed magnetic field of said preparation method;
Constant-temperature temperature-control equipment, said constant-temperature temperature-control equipment is used to regulate and control the needed temperature of said preparation method.
When the present invention implemented, preferably, said magnetic field generating apparatus comprised:
Magnetic field produces power supply;
Two magnetic poles, said two magnetic poles are oppositely arranged, and said two magnetic poles produce power supply with said magnetic field and are connected through lead, and said material platform is arranged between said two magnetic poles.
When the present invention implemented, preferably, said thermostatic control device comprised:
The thermostatically controlled power supply;
Hot-plate, said hot-plate cross a chamber, and said material platform is arranged in the said chamber, and said hot-plate is connected through lead with said thermostatically controlled power supply;
Thermopair, said thermopair are arranged in the said chamber, and said thermopair is connected through lead with said thermostatically controlled power supply.
Beneficial effect of the present invention is following:
1, preparation method of the present invention utilizes field orientation to strengthen to have replaced the assembling effect of template of the prior art, tensio-active agent, organic complexing agent, and no poisonous, obnoxious flavour is emitted environmental protection in the entire reaction course.
2, preparing method's technology of the present invention simple, with low cost, workable, can realize industrialized mass production.
Below will combine accompanying drawing that the technique effect of design of the present invention, concrete structure and generation is described further, so that those skilled in the art understands the object of the invention, characteristic and effect fully.
Description of drawings
Fig. 1 is the structural representation of thermomagnetic treatment device of the present invention;
Fig. 2 is SEM (sem) figure of the NiO nano wire of the embodiment of the invention 1 preparation;
Fig. 3 is XRD (X-ray diffraction) figure of the NiO nano wire of the embodiment of the invention 1 preparation;
Fig. 4 is the SEM figure of the NiO nano wire of the embodiment of the invention 2 preparations;
Fig. 5 is the XRD figure of the NiO nano wire of the embodiment of the invention 2 preparations;
Fig. 6 is the SEM figure of the NiO nano wire of the embodiment of the invention 3 preparations;
Fig. 7 is the XRD figure of the NiO nano wire of the embodiment of the invention 3 preparations;
Fig. 8 is the SEM figure of the NiO nano wire of the embodiment of the invention 4 preparations;
Fig. 9 is the XRD figure of the NiO nano wire of the embodiment of the invention 4 preparations.
Embodiment
As shown in Figure 1, thermomagnetic treatment device of the present invention comprises: material platform 8, magnetic field generating apparatus 1, constant-temperature temperature-control equipment 2 and support 4.
Material platform 8 is used for ccontaining material.
Magnetic field generating apparatus 1 is used for producing and regulating and control the needed magnetic field of preparation method of the present invention.Magnetic field generating apparatus comprises that magnetic field produces power supply 3, two magnetic poles 51,52.Magnetic field produces power supply 3 and is used for to 51,52 power supplies of two magnetic poles to produce magnetic field and to regulate and control magneticstrength; Two magnetic poles 51,52 are oppositely arranged; Two magnetic poles 51,52 and magnetic field produce power supply 3 and are connected through lead, and material platform 8 is arranged on two magnetic poles 51, between 52.
Constant-temperature temperature-control equipment 2 is used to regulate and control the needed temperature of thermomagnetic treatment.Thermostatic control device 2 comprises thermostatically controlled power supply 6, hot-plate 9, thermopair 7.Thermostatically controlled power supply 6 is used for the heating to hot-plate 9 power supply and control hot-plate 9, and hot-plate 9 is arranged on two magnetic poles 51, between 52.Hot-plate 9 crosses a chamber, and material platform 8 is arranged in the chamber, particularly is arranged on the chamber center.Hot-plate 9 and thermostatically controlled power supply 6 are connected through lead.Thermopair 7 is arranged in the chamber, and thermopair 7 and thermostatically controlled power supply 6 are connected through lead.
Support 4 is used for supporting, fixedly material platform 8, hot-plate 9, magnetic pole 51,52.Support 4 is refractory brick supports.Support 4 comprises U type base 41, cushion block 42 and two spacer blocks 431,432.In U type base 41, be provided with cushion block 42, hot-plate 9 is arranged in U type base 41, and is fixed on the cushion block 42.Magnetic pole 51,52 is arranged in U type base 41, hot-plate 9 and magnetic pole 51, is provided with spacer block 431,432 between 52, and so, magnetic pole 51,52 is fixed in the support 4.
A kind of preparation method of NiO nano wire may further comprise the steps:
A) the Ni nano wire being placed as in the described thermomagnetic treatment device of this embodiment, particularly is to place material platform 8;
B) under magneticstrength is the magnetic field environment of 0.05T-0.52T, heat up, the temperature rise rate of intensification is 0.5 ℃/min-50 ℃/min, and intensification is that to be warming up to temperature of charge be 400 ℃-1500 ℃;
C) under magneticstrength is the magnetic field environment of 0.05T-0.52T, be incubated, insulation is that temperature of charge is remained on the temperature of charge after heating up in the step b), and the soaking time of insulation is 1.5h-15h;
D) under magneticstrength is the magnetic field environment of 0.05T-0.52T, carry out naturally cooling,, promptly get the NiO nano wire until room temperature.
Magneticstrength in step b), step c) and the step d) can be identical, also can be different.
The preparation method of NiO nano wire carries out under normal pressure, in the air.
In following examples, the equipment and the correlation parameter that carry out the employing of SEM sign are: the model of Zeiss, Germany company is the sem of Ultra 55, and acceleration voltage is 5kV during test; Carrying out the equipment that XRD characterize to adopt is: the model of German Brooker company is the X-ray diffractometer of D8ADVANCE.
In following examples, used Ni nano wire is commercially available Ni nano wire, to its correlation parameter and unrestricted.
Embodiment 1
The Ni nano wire is placed as in the described thermomagnetic treatment device of this embodiment, and magneticstrength is set at 0.3T, is warming up to 800 ℃ with the speed of 10 ℃/min; Magneticstrength is set at 0.4T then, 800 ℃ of insulation 8h; Last magneticstrength is set at 0.3T, naturally cools to room temperature and gets final product.
SEM photo such as Fig. 2 of the NiO nano wire that makes, XRD test result such as Fig. 3.
Embodiment 2
The Ni nano wire is placed as in the described thermomagnetic treatment device of this embodiment, and magneticstrength is set at 0.52T, is warming up to 400 ℃ with the speed of 0.5 ℃/min; Magneticstrength is set at 0.52T then, 400 ℃ of insulation 15h; Last magneticstrength is set at 0.52T, naturally cools to room temperature and gets final product.
SEM photo such as Fig. 4 of the NiO nano wire that makes, XRD test result such as Fig. 5.
Embodiment 3
The Ni nano wire is placed as in the described thermomagnetic treatment device of this embodiment, and magneticstrength is set at 0.3T, is warming up to 600 ℃ with the speed of 5 ℃/min; Magneticstrength is set at 0.4T then, 600 ℃ of insulation 10h; Last magneticstrength is set at 0.3T, naturally cools to room temperature and gets final product.
SEM photo such as Fig. 6 of the NiO nano wire that makes, XRD test result such as Fig. 7.
Embodiment 4
The Ni nano wire is placed as in the described thermomagnetic treatment device of this embodiment, and magneticstrength is set at 0.1T, is warming up to 1000 ℃ with the speed of 30 ℃/min; Magneticstrength is set at 0.3T then, 1000 ℃ of insulation 5h; Last magneticstrength is set at 0.1T, naturally cools to room temperature and gets final product.
SEM photo such as Fig. 8 of the NiO nano wire that makes, XRD test result such as Fig. 9.
In the XRD figure (Fig. 3,5,7,9) of embodiment 1-4; All be that the peak appears in the position near 37.25 °, 43.28 °, 62.87 °, 75.41 °, 79.40 °, 95.06 °; These peaks corresponding successively (111), (200), (220), (311), (222), (400) peak; And other position Wu Feng shows that prepared what go out is pure NiO crystal.Can find out that by the SEM of embodiment 1-4 figure (Fig. 2,4,6,8) prepared what go out is nano wire.Can conclude that by XRD and SEM figure prepared what go out is the NiO nano wire to embodiment 1-4.
More than describe preferred embodiment of the present invention in detail.The ordinary skill that should be appreciated that this area need not creative work and just can design according to the present invention make many modifications and variation.Therefore, all technician in the art all should be in the determined protection domain by claims under this invention's idea on the basis of existing technology through the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (9)
1. the preparation method of a NiO nano wire is characterized in that, places magnetic field environment to heat-treat the Ni nano wire, to obtain said NiO nano wire.
2. the preparation method of NiO nano wire as claimed in claim 1 is characterized in that, may further comprise the steps:
A) the Ni nano wire is placed magnetic field environment;
B) under magnetic field environment, heat up;
C) under magnetic field environment, be incubated;
D) under magnetic field environment, carry out naturally cooling,, promptly get said NiO nano wire until room temperature.
3. the preparation method of NiO nano wire as claimed in claim 2; It is characterized in that: in said step b); The magneticstrength of said magnetic field environment is 0.05T-0.52T; The temperature rise rate of said intensification is 0.5 ℃/min-50 ℃/min, and said intensification is that to be warming up to temperature of charge be 400 ℃-1500 ℃.
4. the preparation method of NiO nano wire as claimed in claim 2; It is characterized in that: in said step c); The magneticstrength of said magnetic field environment is 0.05T-0.52T, and said insulation is that the maintenance temperature of charge is 400 ℃-1500 ℃, and the soaking time of said insulation is 1.5h-15h.
5. the preparation method of NiO nano wire as claimed in claim 2 is characterized in that: in said step d), the magneticstrength of said magnetic field environment is 0.05T-0.52T.
6. the preparation method of NiO nano wire as claimed in claim 2 is characterized in that: the preparation method of said NiO nano wire carries out under normal pressure, in the air.
7. a thermomagnetic treatment device that is used for the preparation method of the described NiO nano wire of one of claim 1-6 is characterized in that, comprising:
The material platform, said material platform is used for ccontaining material;
Magnetic field generating apparatus, said magnetic field generating apparatus are used for producing and regulating and control the needed magnetic field of said preparation method;
Constant-temperature temperature-control equipment, said constant-temperature temperature-control equipment is used to regulate and control the needed temperature of said preparation method.
8. thermomagnetic treatment device as claimed in claim 7 is characterized in that, said magnetic field generating apparatus comprises:
Magnetic field produces power supply;
Two magnetic poles, said two magnetic poles are oppositely arranged, and said two magnetic poles produce power supply with said magnetic field and are connected through lead, and said material platform is arranged between said two magnetic poles.
9. thermomagnetic treatment device as claimed in claim 7 is characterized in that, said thermostatic control device comprises:
The thermostatically controlled power supply;
Hot-plate, said hot-plate cross a chamber, and said material platform is arranged in the said chamber, and said hot-plate is connected through lead with said thermostatically controlled power supply;
Thermopair, said thermopair are arranged in the said chamber, and said thermopair is connected through lead with said thermostatically controlled power supply.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104313728A (en) * | 2014-10-21 | 2015-01-28 | 南京大学（苏州）高新技术研究院 | Exchange bias nickel-base ferromagnetic/antiferromagnetic composite nano fiber and preparation method thereof |
| CN104313728B (en) * | 2014-10-21 | 2017-01-04 | 南京大学（苏州）高新技术研究院 | Exchange-biased nickel-based ferromagnetic/antiferromagnetic composite nanofiber and preparation method thereof |
| CN111378812A (en) * | 2020-04-08 | 2020-07-07 | 上海大学 | Heat treatment method for improving proportion of metal zigzag grain boundaries and heat treatment system used by heat treatment method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104313728A (en) * | 2014-10-21 | 2015-01-28 | 南京大学（苏州）高新技术研究院 | Exchange bias nickel-base ferromagnetic/antiferromagnetic composite nano fiber and preparation method thereof |
| CN104313728B (en) * | 2014-10-21 | 2017-01-04 | 南京大学（苏州）高新技术研究院 | Exchange-biased nickel-based ferromagnetic/antiferromagnetic composite nanofiber and preparation method thereof |
| CN111378812A (en) * | 2020-04-08 | 2020-07-07 | 上海大学 | Heat treatment method for improving proportion of metal zigzag grain boundaries and heat treatment system used by heat treatment method |
| CN111378812B (en) * | 2020-04-08 | 2021-03-23 | 上海大学 | Heat treatment method for improving proportion of metal zigzag grain boundaries and heat treatment system used by heat treatment method |
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