CN106835366A - A kind of preparation method of cobalt nitride hollow nano fiber - Google Patents
A kind of preparation method of cobalt nitride hollow nano fiber Download PDFInfo
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- CN106835366A CN106835366A CN201710091648.8A CN201710091648A CN106835366A CN 106835366 A CN106835366 A CN 106835366A CN 201710091648 A CN201710091648 A CN 201710091648A CN 106835366 A CN106835366 A CN 106835366A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
Abstract
The present invention relates to a kind of preparation method of cobalt nitride hollow nano fiber, belong to technical field of nanometer material preparation.The present invention prepares Co using electrostatic spinning technique with the method that ammonia nitridation is combined2N hollow nano fibers.The present invention includes four steps：(1) spinning solution is prepared；(2) PVP/Co (NO are prepared3)2Composite nano fiber, is prepared using electrostatic spinning technique；(3) Co is prepared3O4Hollow nano fiber, by being heat-treated PVP/Co (NO3)2It is prepared by composite nano fiber；(4) Co is prepared2N hollow nano fibers, by Co3O4Hollow nano fiber is nitrogenized with ammonia, obtains Co2N hollow nano fibers, with good crystallinity, belong to rhombic system, and a diameter of 73.99 ± 0.55nm, length is more than 30 μm.Preparation method of the invention is simple and easy to apply, can produce in batches, has broad application prospects.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, a kind of preparation of cobalt nitride hollow nano fiber is in particulard relate to
Method.
Background technology
The preparation of inorganic matter nanofiber and hollow nano fiber and property research, are material science, Condensed Matter Physics, change
One of etc. forward position focus research field of subject.Nanofiber refers to have bidimensional to be on the three dimensions yardstick of material to receive
The filamentary material of metrical scale, generally radially yardstick is nanometer scale, and length is then larger.Because the radial dimension of nanofiber is small
To nanometer scale, series of characteristics is shown, most prominent is big specific surface area, so that its surface can increase with activity, and then
Small-size effect, surface or interfacial effect, quantum size effect, macro quanta tunnel effect etc. are produced, and therefore shows one
Specificity in terms of sequence of chemical, physics such as heat, light, sound, electricity, magnetic.Hollow nano fiber is due to bigger specific surface
Product, will be with widely application.In the prior art, there are many methods for preparing nanofiber, method of for example reeling off raw silk from cocoons, template are closed
Cheng Fa, split-phase method and self-assembly method etc..Additionally, also arc evaporation, laser high temperature inustion, compound pyrolysismethod.This
Three kinds of methods are essentially all after making compound or simple substance evaporation at high temperature, through the prepared nanofiber of pyrolysis or directly condensation or
Nanotube, essentially, belongs to compound steam sedimentation.
Cobalt nitride has various compositions, and such as chemical formula is CoN1.2, Co5.47N, Co4N,Co3N,Co2N etc..Cobalt nitride has
Wide application prospect, is such as applied to lithium ion battery, in ultracapacitor, fuel-cell catalyst and Hydrobon catalyst
Deng.The research of nano silicon nitride cobalt has turned into one of focus of material science research.Cobalt nitride nano-powder is had at present
Report, is generally prepared using high temperature gas-solid phase reaction, is such as reacted with nitrogen using metallic cobalt nano-powder, or use cobalt
Salt or oxide prepare cobalt nitride nano-powder with ammonia or nitrogen reaction, but have not yet to see chemical composition for Co2N nitrogen
Change the report of cobalt hollow nano fiber one-dimensional nano structure material.
The United States Patent (USP) of Patent No. 1975504 discloses a relevant electrospinning process (electrospinning)
Technical scheme, the method is to prepare a kind of continuous, effective ways of the micro nanometer fiber with macro length, by
Formhals was proposed first in 1934.This method is mainly used to prepare high polymer nanometer fiber, it is characterized in that making powered
Polymer Solution or melt are sprayed by the traction of electrostatic force in electrostatic field by nozzle, invest the receiving screen on opposite, so that real
Existing wire drawing, then, solvent evaporation, or melt cooling at normal temperatures solidifies to normal temperature, obtains micro nanometer fiber.Nearly 10 years
Come, occurred in that in inorfil preparing technical field and prepare inorganic compound such as oxide nanofiber using electrospinning process
Technical scheme, described oxide includes TiO2、ZrO2、Y2O3、Y2O3:RE3+(RE3+=Eu3+、Tb3+、Er3+、Yb3+/Er3+)、
NiO、Co3O4、Mn2O3、Mn3O4、CuO、SiO2、Al2O3、ZnO、Nb2O5、MoO3、CeO2、LaMO3(M=Fe, Cr, Mn, Co, Ni,
Al)、Y3Al5O12、La2Zr2O7Deng metal oxide and composite oxide of metal.By adjusting the composition of spinning solution, Dong Xiangting etc.
CeO is directly prepared for using electrostatic spinning technique2Hollow nano fiber [Journal ofRare Earths, 2008,26 (5),
664-669]；Wang Jinxian etc. is directly prepared for LaCoO using electrostatic spinning technique3Porous hollow nano fiber
[AppliedPhysics Research,2009,1(1),8-14].Have no at present and nitrogenize phase with ammonia using electrostatic spinning technique
With reference to method prepare Co2The report of N hollow nano fibers.
When preparing nano material using electrostatic spinning technique, the species of raw material, the molecular weight of high polymer templates, spinning solution
Composition, spinning process parameter and Technology for Heating Processing all have a major impact to the pattern and size of final products.The present invention is used
Electrostatic spinning technique and ammonia NH3The method that nitridation is combined prepares Co2N hollow nano fibers.With cabaltous nitrate hexahydrate Co
(NO3)2·6H2O is raw material, adds solvent DMF DMF and ethanol C2H5OH, adds high polymer templates and gathers
Vinylpyrrolidone PVP, electrostatic spinning is carried out after obtaining spinning solution, under optimal experiment condition, prepares PVP/Co (NO3)2
Composite nano fiber, it is heat-treated in atmosphere, obtains Co3O4Hollow nano fiber, will using the ammonia of flowing
Co3O4Hollow nano fiber is nitrogenized, and has prepared the Co of pure phase2N hollow nano fibers.
The content of the invention
Preparation cobalt nitride nano-powder in the introduction, employs high temperature gas-solid phase reaction method.In background technology
Co is prepared for using electrostatic spinning technique3O4Nanofiber and CeO2Deng metallic oxide hollow nano fiber.The original for being used
Material, template, solvent and reducing agent and the method for the present invention are different.In order to provide a kind of in cobalt nitride field of nanometer material technology
New hollow nano fiber one-dimensional nano structure material, we have invented the Co for preparing electrostatic spinning technique3O4Hollow Nano
Used as presoma, it is Co nitridation to be carried out with ammonia and prepares chemical formula to fiber2The method of N cobalt nitride hollow nano fibers.
The present invention is achieved in that the spinning solution with certain viscosity prepared first for electrostatic spinning, application
Electrostatic spinning technique carries out electrostatic spinning, under optimal experiment condition, prepares PVP/Co (NO3)2Composite nano fiber, will
It is heat-treated in atmosphere, obtains Co3O4Hollow nano fiber, then nitrogenized with the ammonia of flowing, prepare structure
The Co of novel pure phase2N hollow nano fibers.Its step is：
(1) spinning solution is prepared
Cobalt source uses cabaltous nitrate hexahydrate Co (NO3)2·6H2O, high polymer templates use polyvinylpyrrolidone
PVP, molecular weight is 90000, using DMF DMF and ethanol C2H5OH is solvent, by 1.0052g Co
(NO3)2·6H2O is added in the mixed solution of 5.0022g DMF and 5.0022g ethanol, is added after magnetic agitation dissolving
1.0031g PVP, continue stirring 10h and obtain transparent spinning solution；
(2) PVP/Co (NO are prepared3)2Composite nano fiber
Spinning solution is injected in a 10mL syringe with 1mL plastic spray gun heads, during graphite rod inserted into spinning solution,
The positive terminal of graphite rod and high-voltage DC power supply is connected with copper cash, the earth terminal of high-voltage DC power supply is put with vertical
The wire netting copper cash put is connected and is grounded, wire netting as composite nano fiber reception device, lance head and horizontal plane
Angle is 15 °, and lance head is 17cm with the spacing of receiving screen wire netting, and spinning voltage is 14kV, and indoor temperature is 20-30 DEG C,
Relative humidity is 20%-50%, carries out electrostatic spinning and obtains PVP/Co (NO3)2Composite nano fiber；
(3) Co is prepared3O4Hollow nano fiber
By described PVP/Co (NO3)2Composite nano fiber is heat-treated in being put into temperature programmed control Muffle furnace, with 1 DEG C/
The heating rate of min rises to 380 DEG C and is incubated 2h, is down to 200 DEG C with the rate of temperature fall of 1 DEG C/min afterwards, then with body of heater certainly
Room temperature so is cooled to, Co is obtained3O4Hollow nano fiber；
(4) Co is prepared2N hollow nano fibers
By described Co3O4Hollow nano fiber is placed in quartz boat, is placed into vacuum tube furnace, first uses vacuum pumping
Go out furnace air, then pass to ammonia, rise to 350 DEG C with the heating rate of 1 DEG C/min and be incubated 6h, afterwards with 1 DEG C/min's
Rate of temperature fall is down to 100 DEG C, then naturally cools to room temperature with body of heater, obtains Co2N hollow nano fibers, a diameter of 73.99 ±
0.55nm, length is more than 30 μm.
Described Co in above process2N hollow nano fibers have good crystallinity, belong to rhombic system, diameter
It is 73.99 ± 0.55nm, length is more than 30 μm, realizes goal of the invention.
Brief description of the drawings
Fig. 1 is PVP/Co (NO3)2The SEM photograph of composite nano fiber；
Fig. 2 is PVP/Co (NO3)2The diameter distribution histogram of composite nano fiber；
Fig. 3 is Co3O4The XRD spectra of hollow nano fiber；
Fig. 4 is Co3O4The SEM photograph of hollow nano fiber；
Fig. 5 is Co3O4The diameter distribution histogram of hollow nano fiber；
Fig. 6 is Co3O4The EDS spectrograms of hollow nano fiber；
Fig. 7 is Co3O4The TEM photos of hollow nano fiber；
Fig. 8 is Co2The XRD spectra of N hollow nano fibers；
Fig. 9 is Co2The SEM photograph of N hollow nano fibers, the figure doubles as Figure of abstract；
Figure 10 is Co2The diameter distribution histogram of N hollow nano fibers；
Figure 11 is Co2The EDS spectrograms of N hollow nano fibers；
Figure 12 is Co2The TEM photos of N hollow nano fibers.
Specific embodiment
Cabaltous nitrate hexahydrate Co (NO selected by the present invention3)2·6H2O, molecular weight is 90000 polyvinylpyrrolidone
PVP, ammonia, DMF DMF and ethanol are commercially available analysis net product；Glass apparatus used, crucible and set
Standby is the instrument and equipment commonly used in laboratory.
Embodiment：By 1.0052g Co (NO3)2·6H2The mixing that O is added to 5.0022g DMF and 5.0022g ethanol is molten
In liquid, 1.0031g PVP are added after magnetic agitation dissolving, continue stirring 10h and obtain transparent spinning solution；Spinning solution is injected
In one 10mL syringe with 1mL plastic spray gun heads, by graphite rod insertion spinning solution, graphite rod and height are connected with copper cash
The positive terminal of dc source is pressed, the earth terminal of high-voltage DC power supply is connected with the wire netting being disposed vertically with copper cash
And be grounded, wire netting as composite nano fiber reception device, the angle of lance head and horizontal plane is 15 °, lance head with connect
The spacing for receiving screen wire netting is 17cm, and spinning voltage is 14kV, and indoor temperature is 20-30 DEG C, and relative humidity is 20%-50%,
Carry out electrostatic spinning and obtain PVP/Co (NO3)2Composite nano fiber；By described PVP/Co (NO3)2Composite nano fiber is put into
It is heat-treated in temperature programmed control Muffle furnace, rises to 380 DEG C with the heating rate of 1 DEG C/min and be incubated 2h, afterwards with 1 DEG C/min
Rate of temperature fall be down to 200 DEG C, then naturally cool to room temperature with body of heater, obtain Co3O4Hollow nano fiber；Will be described
Co3O4Hollow nano fiber is placed in quartz boat, in placing into vacuum tube furnace, first with vacuum pumped furnace air, Ran Houtong
Enter ammonia, rise to 350 DEG C with the heating rate of 1 DEG C/min and be incubated 6h, be down to 100 DEG C with the rate of temperature fall of 1 DEG C/min afterwards,
Then room temperature is naturally cooled to body of heater, obtains Co2N hollow nano fibers.Described PVP/Co (NO3)2Composite nano fiber has
There is good fiber morphology, fiber surface is smooth, and diameter is evenly distributed, as shown in Figure 1；With Shapiro-Wilk methods to PVP/
Co(NO3)2The diameter of composite nano fiber carries out normal distribution-test, and under 95% confidence level, diameter distribution belongs to normal state point
Cloth, a diameter of 213.14 ± 1.20nm, as shown in Figure 2；Described Co3O4Hollow nano fiber has good crystallinity, and it spreads out
Penetrate the d values and relative intensity and Co at peak3O4PDF standard cards (65-3103) listed by d values it is consistent with relative intensity, belong to vertical
Prismatic crystal system, as shown in Figure 3；Described Co3O4Hollow nano fiber has good hollow nano fiber pattern, and diameter distribution is equal
Even, length is more than 50 μm, as shown in Figure 4；With Shapiro-Wilk methods to Co3O4The diameter of hollow nano fiber carries out normal state
Distribution inspection, under 95% confidence level, diameter is distributed and belongs to normal distribution, a diameter of 83.09 ± 0.49nm, as shown in Figure 5；
Described Co3O4Hollow nano fiber is made up of Co and O elements, Pt from SEM test when sample surfaces plating Pt conductive layers,
Double faced adhesive tapes of a small amount of C used by, as shown in Figure 6；Described Co3O4Hollow nano fiber has obvious hollow-core construction,
As shown in Figure 7；Described Co2N hollow nano fibers have good crystallinity, the d values and relative intensity and Co of its diffraction maximum2N
PDF standard cards (72-1368) listed by d values it is consistent with relative intensity, belong to rhombic system, as shown in Figure 8；Described
Co2N hollow nano fibers have good hollow nano fiber pattern, and diameter is evenly distributed, and length is more than 30 μm, sees Fig. 9 institutes
Show；With Shapiro-Wilk methods to Co2The diameter of N hollow nano fibers carries out normal distribution-test, in 95% confidence level
Under, diameter is distributed and belongs to normal distribution, a diameter of 73.99 ± 0.55nm, as shown in Figure 10；Described Co2N hollow nano fibers
Be made up of Co and N element, Pt from SEM test when sample surfaces plating Pt conductive layers, a small amount of C is from used two-sided
Glue, as shown in Figure 11；Described Co2N hollow nano fibers have obvious hollow-core construction, as shown in Figure 12.
Certainly, the present invention can also have other various embodiments, ripe in the case of without departing substantially from spirit of the invention and its essence
Know those skilled in the art and work as and various corresponding changes and deformation, but these corresponding changes and change can be made according to the present invention
Shape should all belong to the protection domain of appended claims of the invention.
Claims (2)
1. a kind of preparation method of cobalt nitride hollow nano fiber, it is characterised in that nitrogenized with ammonia using electrostatic spinning technique
The method being combined, is high polymer templates using polyvinylpyrrolidone PVP, using DMF DMF and second
Alcohol is solvent, prepares product for cobalt nitride Co2N hollow nano fibers, its step is：
(1) spinning solution is prepared
Cobalt source uses cabaltous nitrate hexahydrate Co (NO3)2·6H2O, using DMF DMF and ethanol C2H5OH
It is solvent, by 1.0052g Co (NO3)2·6H2O is added in the mixed solution of 5.0022g DMF and 5.0022g ethanol, magnetic force
1.0031g PVP are added after stirring and dissolving, is continued stirring 10h and is obtained transparent spinning solution；
(2) PVP/Co (NO are prepared3)2Composite nano fiber
Spinning solution is injected in a 10mL syringe with 1mL plastic spray gun heads, by graphite rod insertion spinning solution, copper is used
Line connects the positive terminal of graphite rod and high-voltage DC power supply, by the earth terminal of high-voltage DC power supply be disposed vertically
Wire netting copper cash is connected and is grounded, wire netting as composite nano fiber reception device, the angle of lance head and horizontal plane
It it is 15 °, lance head is 17cm with the spacing of receiving screen wire netting, spinning voltage is 14kV, and indoor temperature is 20-30 DEG C, relatively
Humidity is 20%-50%, carries out electrostatic spinning and obtains PVP/Co (NO3)2Composite nano fiber；
(3) Co is prepared3O4Hollow nano fiber
By described PVP/Co (NO3)2Composite nano fiber is heat-treated in being put into temperature programmed control Muffle furnace, with 1 DEG C/min's
Heating rate rises to 380 DEG C and is incubated 2h, is down to 200 DEG C with the rate of temperature fall of 1 DEG C/min afterwards, then with body of heater natural cooling
To room temperature, Co is obtained3O4Hollow nano fiber；
(4) Co is prepared2N hollow nano fibers
By described Co3O4Hollow nano fiber is placed in quartz boat, in placing into vacuum tube furnace, first with vacuum pumped stove
Interior air, then passes to ammonia, rises to 350 DEG C with the heating rate of 1 DEG C/min and is incubated 6h, afterwards with the cooling of 1 DEG C/min
Speed is down to 100 DEG C, then naturally cools to room temperature with body of heater, obtains Co2N hollow nano fibers, a diameter of 73.99 ±
0.55nm, length is more than 30 μm.
2. a kind of preparation method of cobalt nitride hollow nano fiber according to claim 1, it is characterised in that high score submodule
Plate agent is the polyvinylpyrrolidone of molecular weight Mr=90000.
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Cited By (2)
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| CN109742350A (en) * | 2018-12-28 | 2019-05-10 | 上海应用技术大学 | A kind of ferroso-ferric oxide/graphene composite material preparation method of nitridation |
| CN111063888A (en) * | 2019-12-11 | 2020-04-24 | 肇庆市华师大光电产业研究院 | Preparation method of modified carbon nanofiber lithium-sulfur battery positive electrode material |
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