CN107117589B - A kind of high specific capacitance (BC) xNyOz material and its synthetic method - Google Patents
A kind of high specific capacitance (BC) xNyOz material and its synthetic method Download PDFInfo
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- CN107117589B CN107117589B CN201710378559.1A CN201710378559A CN107117589B CN 107117589 B CN107117589 B CN 107117589B CN 201710378559 A CN201710378559 A CN 201710378559A CN 107117589 B CN107117589 B CN 107117589B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/0828—Carbonitrides or oxycarbonitrides of metals, boron or silicon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The present invention provides a kind of high specific capacitance (BC)xNyOzUltrasonic dissolution in solvent is added in raw material containing B respectively and raw material containing CN by material and its synthetic method, including (1), pre-processes mixed solution；(2) above-mentioned mixed solution is mixed with catalyst, is put into closed reaction kettle, heated cooling obtains crude product in solution；(3) solid in above-mentioned crude product in solution is isolated, two sections of heating obtain crude product powder to be fully ground after removing solvent and excessive moisture under rare gas protection；(4) above-mentioned crude product powder is washed with acid and deionized water, obtains (BC)xNyOzMaterial, wherein 3≤x≤9,0.5≤y≤1,0≤z≤9.
Description
Technical field
The present invention relates to a kind of high specific capacitance (BC)xNyOzMaterial and its synthetic method.
Background technique
Due to C and BN structure and in terms of similitude, and because their certain physical properties exist it is very big
Difference, obtain a kind of new material with performances such as special power, heat, electricity, light it is intended that combining both.Tool
The novel tertiary BCN material of standby two kinds of material advantages comes into being.People usually regard such ternary BCN material as graphite network
The product that middle part carbon atom is replaced by boron or nitrogen-atoms, though morphosis has similarity with carbon nanotube, it has
Mechanical performance more superior than carbon nanotube and electric property, and influence of its diameter to its mechanical performance and electric property is very
It is small.Therefore, (BC)xNyOzMaterial has widely in composite material, magnetic material, luminescent material and electronic material numerous areas
Application prospect.
(although BC)xNyOzMaterial has many advantageous properties, but the bottleneck for restricting its application is that its preparation is difficult, closes
It is lower at yield, and synthesis process is difficult to control.In the prior art, (BC) is preparedxNyOzThe main method of material has electric arc to put
Electrical method, plasma evaporation method, heated filament vapour deposition process and high temperature and high pressure method etc., and under different preparation conditions, it prepares
The boron carbon nitrogen trielement compound or boron carbon oxynitride that come in every shape different with Elemental redistribution.Wherein high temperature and high pressure method is most
It with this method, is had been realized in for example: the industrialization of cubic boron nitride so far for maturation.But comprehensive analysis
This method is not difficult to find out, preparation process, which still needs, uses extreme condition, such as temperature is higher than at 1000 DEG C also needs Manual pressurizing,
Very harsh requirement is thus proposed to equipment, this is directly resulted in device requirement height, and product price is high；In addition,
With the preparation method of high temperature and pressure, its product defect is more, and crystallite size adjustable extent is narrow, so that the specific capacitance of product is difficult to reach
The range stable to one is limited in terms of it is applied to supercapacitor storage charge material.
The research of forefathers is concentrated mainly on the BC that C and BN has stoichiometric2N compound.Theoretically, pass through change
C, the proportion of B, N, the proportion of even addition O, can be designed the BCN material or BCNO material of different component.With technology of preparing
Progress, develop (BC) that a kind of mild, easy to operate, the at low cost synthetic method of reaction condition prepares high specific capacitancexNyOzMaterial
Material just has great importance.
Summary of the invention
It is an object of the invention to provide a kind of high specific capacitance (BC) in place of overcome the deficiencies in the prior artxNyOzMaterial
Material and its synthetic method, solve above-mentioned background technique high temperature high pressure, preparation condition harshness, complex process, product specific capacitance
The problems such as unstable.
The technical solution adopted by the present invention to solve the technical problems is: providing a kind of high specific capacitance (BC)xNyOzMaterial
The synthetic method of material, includes the following steps:
(1) it pre-processes mixed solution: B raw material will be contained and raw material containing CN is added in solvent and carries out ultrasonic dissolution, mixed
Solution；The raw material containing B includes sodium borohydride, nano boron powder, boric acid, potassium borohydride；The raw material containing CN include melamine,
1,3,5- s-triazine, pyrazine, 2,4,6- tri- (2- pyridyl group) triazines, Cyanuric Chloride；
(2) it prepares crude product in solution: above-mentioned mixed solution being mixed with catalyst, is put into closed reaction kettle, in temperature
Degree is to heat 5-30h at 150-250 DEG C, through cooled to room temperature, obtains crude product in solution；
(3) it prepares crude product powder: isolating the solid in above-mentioned crude product in solution, add for two sections under rare gas protection
Heat, first segment heating temperature are 100-300 DEG C, heating time 1-2h, and second segment heating temperature is 700-900 DEG C, when heating
Between be 1-2h, will heating remove excessive moisture solid be fully ground, obtain crude product powder；
(4) (BC) is preparedxNyOzMaterial: it is the above-mentioned crude product powder of 2-6 acid elution with pH value, is later 30-80 with temperature
DEG C deionized water wash 1-10 times；By the product after washing 30-100 DEG C at a temperature of dry, obtain (BC)xNyOzMaterial,
Wherein 3≤x≤9,0.5≤y≤1,0≤z≤9.
In a preferred embodiment of the present invention, the solvent includes water, ammonium hydroxide, ethylenediamine, ethyl alcohol, ethylene glycol, acetonitrile.
In a preferred embodiment of the present invention, the catalyst includes Co, Ni, Fe.
The present invention also provides a kind of high specific capacitance (BC)xNyOzMaterial, it is described (BC)xNyOzMaterial, wherein 3≤x≤9,
0.5≤y≤1, (BC) described in 0≤z≤9xNyOzScantling is 1-10 μm, specific capacitance 400-1000F/g.
It is described (BC) in a preferred embodiment of the present inventionxNyOzMaterial be the flake being stacked with, fold it is spherical or
It is brilliant Filamentous.
The technical program compared with the background art, it has the following advantages:
1. synthetic method of the invention is not necessarily to external pressurized, preparation temperature is low, and reaction condition is mild；
2. synthetic method raw material of the invention is taken simply, without doing excessive pretreatment or preparing presoma, technique letter
It is single；
3.B, C and N atom are dissolved in catalyst metal particles, spread and are precipitated, so that it is with stable crystal form；It urges
The application of agent reduces the phenomenon that B, C, N reunite in the liquid phase after by van der Waals interaction, keeps product dispersion effect good, purifies
Convenient, size is controllable；
4. product (BC) of the inventionxNyOzMaterial, wherein 3≤x≤9,0.5≤y≤1,0≤z≤9, have stable and high
Specific capacitance, value can reach 400-1000F/g.
Detailed description of the invention
Fig. 1 depicts the stereoscan photograph that the embodiment of the present invention 1 prepares sample；
Fig. 2 depicts the cyclic voltammetry curve that the embodiment of the present invention 1 prepares sample；
Fig. 3 depicts the charging and discharging curve that the embodiment of the present invention 1 prepares sample；
Fig. 4 depicts the infrared spectrogram that the embodiment of the present invention 2 prepares sample；
Fig. 5 depicts the stereoscan photograph that the embodiment of the present invention 3 prepares sample；
Fig. 6 depicts the stereoscan photograph that the embodiment of the present invention 4 prepares sample；
Fig. 7 depicts the stereoscan photograph that the embodiment of the present invention 5 prepares sample；
Specific embodiment
The contents of the present invention are illustrated below with reference to embodiment and attached drawing:
Embodiment 1
A kind of high specific capacitance (BC)xNyOzThe synthetic method of material, includes the following steps:
(1) it pre-processes mixed solution: boric acid and (2- pyridyl group) triazine of 2,4,6- tri- being added in ethylene glycol solvent and carried out
Ultrasonic dissolution 5min, obtains mixed solution；The formula rate of said components is 3.5g:1g:10ml.
(2) it prepares crude product in solution: above-mentioned mixed solution is transferred in reaction kettle, suitable nickel foam conduct is added and urges
Agent, locking reaction kettle are put into baking oven, and the temperature that baking oven is arranged is 250 DEG C, are heated cooled to room temperature after 24 h, are taken out
Reaction kettle obtains crude product in solution；
(3) it prepares crude product powder: above-mentioned crude product in solution is centrifugated, the solid isolated is transferred to aluminium oxide
In porcelain boat, aluminium oxide porcelain boat is placed in tube furnace, heating is under the protection of nitrogen to remove residual solvent:
First segment heating temperature is 250 DEG C, heating time 1h；
Second segment heating temperature is 800 DEG C, heating time 2h；
Aluminium oxide porcelain boat is taken out later, collects remaining solid powder, is ground sufficiently in mortar, is obtained crude product powder
End；
(4) (BC) is preparedxNyOzMaterial: it is the above-mentioned crude product powder of 5 salt acid elutions with pH value, removes catalyst, Zhi Houyong
The deionized water washed product that temperature is 50 DEG C removes the salt and the complete raw material of unreacted contained in product, washing times 5-
10 times；By the product after washing 50-100 DEG C at a temperature of dry, obtain sample (BC)xNyOzMaterial, wherein x=6.3, y=
1, z=7.3.
With Fourier Transform Infrared Spectrometer (Nicolet iS50) and x-ray photoelectron spectroscopy (Thermo
ESCALAB 250) sample prepared by the present embodiment method is tested, test result shows to contain B-N, B-C, B-C-N in sample
Key illustrates product not and is simply physical mixture, formed the bonding in atomic level.
Fig. 1 is please referred to, the present embodiment sample is observed on scanning electron microscope (Hitachi-SU8000), it can be seen that
The laminar sample being stacked with, 1-10 μm of size range.
Fig. 2 and Fig. 3 are please referred to, (electric current is close with the specific capacitance of electrochemical workstation (CHI760E) test the present embodiment sample
Degree is 0.5A/g), as shown, being calculated with formula Cm=I Δ t/m Δ v, specific capacitance 931.5F/g.
Embodiment 2
Fig. 4 is please referred to, the present embodiment is matched the difference from embodiment 1 is that the solvent is changed to ethylenediamine by ethylene glycol
Than constant, sample (BC) is obtainedxNyOzMaterial, wherein x=4, y=1, z=5.Infrared spectrogram is carried out for the present embodiment sample
Spectrum analysis finds that there are corresponding B-N, B-C, B-C-N keys in sample.Illustrate that product has formed bonding in atomic level.
Embodiment 3
The present embodiment is the difference from embodiment 1 is that the catalyst changes into Co powder by nickel foam (Ni).For this reality
It applies a sample to be analyzed, please refers to Fig. 5, the present embodiment sample is observed on scanning electron microscope (Hitachi-SU8000)
Product, discovery synthesize the spherical product of fold, and catalyst influences product shape.
Embodiment 4
The present embodiment the difference from embodiment 1 is that:
(1) it pre-processes mixed solution: boric acid and pyrazine being added in acetonitrile solvent and carry out ultrasonic dissolution 5min, is mixed
Solution；The formula rate of said components is 3.1g:1g:10ml.
Remaining step is same as Example 1, obtains sample (BC)xNyOzMaterial, wherein x=3, y=1, z=1, have found sample
The percentage composition of C, N increased in product.Fig. 6 is please referred to, is observed on scanning electron microscope (Hitachi-SU8000)
The present embodiment sample, it can be seen that laminar sample.
Embodiment 5
A kind of high specific capacitance (BC)xNyOzThe synthetic method of material, includes the following steps:
(1) it pre-processes mixed solution: sodium borohydride and (2- pyridyl group) triazine of 2,4,6- tri- is added in ethylenediamine solvent
Ultrasonic dissolution 5min is carried out, mixed solution is obtained；The formula rate of said components is 2.1g:1g:10ml.
(2) it prepares crude product in solution: above-mentioned mixed solution is transferred in reaction kettle, suitable nickel foam conduct is added and urges
Agent, locking reaction kettle are put into baking oven, and the temperature that baking oven is arranged is 150 DEG C, after heating 7h, are warming up to 250 DEG C, heating
17h, cooled to room temperature, takes out reaction kettle, obtains crude product in solution later；
(3) it prepares crude product powder: above-mentioned crude product in solution is centrifugated, the solid isolated is transferred to aluminium oxide
In porcelain boat, aluminium oxide porcelain boat is placed in tube furnace, heating is under the protection of nitrogen to remove residual solvent:
First segment heating temperature is 250 DEG C, heating time 1h；
Second segment heating temperature is 800 DEG C, heating time 2h；
Aluminium oxide porcelain boat is taken out later, collects remaining solid powder, is ground sufficiently in mortar, is obtained crude product powder
End；
(4) (BC) is preparedxNyOzMaterial: it is the above-mentioned crude product powder of 5 salt acid elutions with pH value, removes catalyst, Zhi Houyong
The deionized water washed product that temperature is 50 DEG C removes the salt and the complete raw material of unreacted contained in product, washing times 5-
10 times；By the product after washing 50-100 DEG C at a temperature of dry, obtain sample (BC)xNyOzMaterial, wherein x=8, y=1,
Z=8.
Fig. 7 is please referred to, the present embodiment sample is observed on scanning electron microscope (Hitachi-SU8000) and synthesizes crystalline substance
Filamentous product.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with scope of protection of the claims
Subject to.
Claims (2)
1. a kind of high specific capacitance (BC)xNyOzThe synthetic method of material, it is characterised in that include the following steps:
(1) it pre-processes mixed solution: B raw material will be contained and raw material containing CN is added in solvent and carries out ultrasonic dissolution, obtain mixed solution；
The raw material containing B is sodium borohydride, nano boron powder, boric acid or potassium borohydride；The raw material containing CN is melamine, 1,3,5- is equal
Triazine, pyrazine, 2,4,6- tri- (2- pyridyl group) triazines or Cyanuric Chloride；
(2) it prepares crude product in solution: above-mentioned mixed solution being mixed with catalyst, is put into closed reaction kettle, is in temperature
5-30h is heated at 150-250 DEG C, through cooled to room temperature, obtains crude product in solution；Wherein, the catalyst be Co, Ni or
Fe；
(3) it prepares crude product powder: isolating the solid in above-mentioned crude product in solution, two sections of heating under rare gas protection,
First segment heating temperature is 100-300 DEG C, heating time 1-2h, and second segment heating temperature is 700-900 DEG C, and heating time is
1-2h is then fully ground, and crude product powder is obtained；
(4) (BC) is preparedxNyOzMaterial: it is the above-mentioned crude product powder of 2-6 acid elution with pH value, is later 30-80 DEG C with temperature
Deionized water is washed 1-10 times；By the product after washing 30-100 DEG C at a temperature of dry, obtain (BC)xNyOzMaterial, wherein
3≤x≤9,0.5≤y≤1,0≤z≤9.
2. a kind of high specific capacitance (BC) according to claim 1xNyOzThe synthetic method of material, it is characterised in that: described molten
Agent is water, ammonium hydroxide, ethylenediamine, ethyl alcohol, ethylene glycol or acetonitrile.
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