CN107117589A - A kind of high specific capacitance (BC) xNyOz materials and its synthetic method - Google Patents
A kind of high specific capacitance (BC) xNyOz materials and its synthetic method Download PDFInfo
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- CN107117589A CN107117589A CN201710378559.1A CN201710378559A CN107117589A CN 107117589 A CN107117589 A CN 107117589A CN 201710378559 A CN201710378559 A CN 201710378559A CN 107117589 A CN107117589 A CN 107117589A
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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 invention provides a kind of high specific capacitance (BC)xNyOzRaw material containing B respectively and raw material containing CN are added ultrasonic dissolution in solvent by material and its synthetic method, including (1), pre-process mixed solution；(2) above-mentioned mixed solution is mixed with catalyst, be put into closed reactor, 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, obtained (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 technology
Due to similitudes of the C and BN in terms of structure and phase transformation law, and because their some physical properties are present greatly
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 materials of standby two kinds of material advantages arise at the historic moment.People generally regard such ternary BCN materials as graphite network
The product that middle part carbon atom is replaced by boron or nitrogen-atoms, though its morphosis has similarity with CNT, it has
The mechanical performance more excellent than CNT 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, magnetic material, luminescent material and electronic material numerous areas
Application prospect.
Although (BC)xNyOzMaterial has many advantageous properties, but restricts bottleneck of its application to be that its is prepared difficult, closes
It is relatively low into yield, and building-up process is difficult to control to.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, prepare
The boron carbon nitrogen trielement compound or boron carbon oxynitride for coming in every shape different with Elemental redistribution.Wherein high temperature and high pressure method is most
For maturation, so far, profit in this way, has been realized in for example：The industrialization of cubic boron nitride.But, comprehensive analysis
This method is not difficult to find out that preparation process, which still needs, uses extreme condition, and such as temperature, which 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 remains high；In addition,
With the preparation method of HTHP, its product defect is more, and crystallite size adjustable extent is narrow, so that the specific capacitance of product is difficult to reach
To a stable scope, it is limited in terms of it is applied to ultracapacitor storage charge material.
The research of forefathers, which is concentrated mainly on C and BN, has the BC of stoichiometric2N compounds.In theory, by changing
C, B, N proportioning, the proportioning for even adding O, can design the BCN materials or BCNO materials of different component.With technology of preparing
Progress, develop (BC) that a kind of synthetic method that reaction condition is gentle, simple to operate, cost is low prepares high specific capacitancexNyOzMaterial
Material just has great importance.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art part, there is provided a kind of high specific capacitance (BC)xNyOzMaterial
And its synthetic method, solve above-mentioned background technology high temperature high pressure, preparation condition harshness, complex process, product specific capacitance not
Stable the problems such as.
The technical solution adopted for the present invention to solve the technical problems is：There is provided a kind of high specific capacitance (BC)xNyOzMaterial
Synthetic method, comprise the following steps：
(1) mixed solution is pre-processed：B raw materials will be contained and raw material containing CN adds 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- pyridine radicals) triazines, Cyanuric Chloride；
(2) crude product in solution is prepared：Above-mentioned mixed solution is mixed with catalyst, is put into closed reactor, in temperature
Spend to heat 5-30h at 150-250 DEG C, through naturally cooling to room temperature, obtain crude product in solution；
(3) crude product powder is prepared：The solid in above-mentioned crude product in solution is isolated, two sections add under rare gas protection
Heat, first paragraph heating-up temperature is 100-300 DEG C, and the heat time is 1-2h, and second segment heating-up temperature is 700-900 DEG C, during heating
Between be 1-2h, by heat 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 elutions with pH value, is afterwards 30-80 with temperature
DEG C deionized water wash 1-10 times；Product after washing is dried at a temperature of 30-100 DEG C, obtained (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, ammoniacal liquor, ethylenediamine, ethanol, ethylene glycol, acetonitrile.
In a preferred embodiment of the present invention, the catalyst includes Co, Ni, Fe.
Present invention also offers a kind of high specific capacitance (BC)xNyOzMaterial, (BC)xNyOzMaterial, wherein 3≤x≤9,
(BC) described in 0.5≤y≤1,0≤z≤9xNyOzScantling is 1-10 μm, and specific capacitance is 400-1000F/g.
In a preferred embodiment of the present invention, (BC)xNyOzMaterial be the flake that is stacked with, fold it is spherical or
It is brilliant thread.
The technical program is compared with background technology, and it has the following advantages that：
1. the synthetic method of the present invention is without external pressurized, preparation temperature is low, and reaction condition is gentle；
2. the synthetic method raw material of the present invention is taken simply, excessive pretreatment or presoma is prepared without doing, technique is simple
It is single；
3.B, C and N atom dissolve in catalyst metal particles, spread and separated out so that it has stable crystal formation；Urge
The application of agent reduces B, C, N by the phenomenon reunited in the liquid phase after van der Waals interaction, makes product dispersion effect good, purification
Convenient, size is controllable；
4. the product (BC) of the present inventionxNyOzMaterial, wherein 3≤x≤9,0.5≤y≤1,0≤z≤9, with stable and high
Specific capacitance, its value can reach 400-1000F/g.
Brief description of the drawings
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；
Embodiment
Present disclosure is illustrated with reference to embodiment and accompanying drawing：
Embodiment 1
A kind of high specific capacitance (BC)xNyOzThe synthetic method of material, comprises the following steps：
(1) mixed solution is pre-processed：Boric acid and 2,4,6- tri- (2- pyridine radicals) triazine are 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) crude product in solution is prepared：Above-mentioned mixed solution is transferred in reactor, appropriate nickel foam is added as urging
Agent, locking reactor is put into baking oven, and the temperature for setting baking oven is 250 DEG C, is naturally cooled to room temperature after heating 24h, is taken out
Reactor, obtains crude product in solution；
(3) crude product powder is prepared：Above-mentioned crude product in solution is centrifuged, the solid isolated is transferred to aluminum oxide
In porcelain boat, aluminum oxide porcelain boat is placed in tube furnace, heats to remove residual solvent under the protection of nitrogen：
First paragraph heating-up temperature is 250 DEG C, and the heat time is 1h；
Second segment heating-up temperature is 800 DEG C, and the heat time is 2h；
Aluminum oxide porcelain boat is taken out afterwards, remaining solid powder is collected, and is ground abundant 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
Temperature is 50 DEG C of deionized water washed product, removes the salt and the complete raw material of unreacted contained in product, washing times are 5-
10 times；Product after washing is dried at a temperature of 50-100 DEG C, sample (BC) is obtainedxNyOzMaterial, wherein x=6.3, y=
1, z=7.3.
With FTIS (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 key in sample,
It is not simply physical mixture, the bonding formed in atomic level to illustrate product.
Fig. 1 is refer to, the present embodiment sample is observed in SEM (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 refer to, (electric current is close with the specific capacitance of electrochemical workstation (CHI760E) test the present embodiment sample
Spend for 0.5A/g), as illustrated, being calculated with formula Cm=I Δ t/m Δs v, specific capacitance is 931.5F/g.
Embodiment 2
Fig. 4 is refer to, the present embodiment and the difference of embodiment 1 are that the solvent is changed to ethylenediamine by ethylene glycol, matched somebody with somebody
Than constant, sample (BC) is obtainedxNyOzMaterial, wherein x=4, y=1, z=5.Infrared spectrogram is carried out for the present embodiment sample
Analysis of spectrum, finds there is corresponding B-N, B-C, B-C-N key in sample.Illustrate that product has formed bonding in atomic level.
Embodiment 3
The present embodiment and the difference of embodiment 1 are that the catalyst changes into Co powder by nickel foam (Ni).For this reality
Apply a sample to be analyzed, refer to Fig. 5, the present embodiment sample is observed in SEM (Hitachi-SU8000)
Product, discovery synthesizes the spherical product of fold, catalyst influence product shape.
Embodiment 4
The present embodiment and the difference of embodiment 1 are：
(1) mixed solution is pre-processed：Boric acid and pyrazine are added ultrasonic dissolution 5min is carried out in acetonitrile solvent, 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, find sample
C, N percentage composition increased in product.Fig. 6 is refer to, is observed in SEM (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, comprises the following steps：
(1) mixed solution is pre-processed：Sodium borohydride and 2,4,6- tri- (2- pyridine radicals) triazine are 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) crude product in solution is prepared：Above-mentioned mixed solution is transferred in reactor, appropriate nickel foam is added as urging
Agent, locking reactor is put into baking oven, and the temperature for setting baking oven is 150 DEG C, after heating 7h, is warming up to 250 DEG C, is heated 17h,
Room temperature is naturally cooled to afterwards, is taken out reactor, is obtained crude product in solution；
(3) crude product powder is prepared：Above-mentioned crude product in solution is centrifuged, the solid isolated is transferred to aluminum oxide
In porcelain boat, aluminum oxide porcelain boat is placed in tube furnace, heats to remove residual solvent under the protection of nitrogen：
First paragraph heating-up temperature is 250 DEG C, and the heat time is 1h；
Second segment heating-up temperature is 800 DEG C, and the heat time is 2h；
Aluminum oxide porcelain boat is taken out afterwards, remaining solid powder is collected, and is ground abundant 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
Temperature is 50 DEG C of deionized water washed product, removes the salt and the complete raw material of unreacted contained in product, washing times are 5-
10 times；Product after washing is dried at a temperature of 50-100 DEG C, sample (BC) is obtainedxNyOzMaterial, wherein x=8, y=1,
Z=8.
Fig. 7 is refer to, the present embodiment sample is observed in SEM (Hitachi-SU8000) and synthesizes crystalline substance
Thread product.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, the change or replacement that can be readily occurred in,
It should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with scope of the claims
It is defined.
Claims (7)
1. a kind of high specific capacitance (BC)xNyOzThe synthetic method of material, it is characterised in that comprise the following steps：
(1) mixed solution is pre-processed：B raw materials will be contained and raw material containing CN adds in solvent and carries out ultrasonic dissolution, mixed solution is obtained；
The raw material containing B includes sodium borohydride, nano boron powder, boric acid, potassium borohydride；The raw material containing CN includes melamine, 1,3,
5- s-triazine, pyrazine, 2,4,6- tri- (2- pyridine radicals) triazines, Cyanuric Chloride；
(2) crude product in solution is prepared：Above-mentioned mixed solution is mixed with catalyst, is put into closed reactor, is in temperature
5-30h is heated at 150-250 DEG C, through naturally cooling to room temperature, crude product in solution is obtained；
(3) crude product powder is prepared：The solid in above-mentioned crude product in solution is isolated, two sections of heating under rare gas protection,
First paragraph heating-up temperature is 100-300 DEG C, and the heat time is 1-2h, and second segment heating-up temperature is 700-900 DEG C, and the heat time is
1-2h, is then fully ground, and obtains crude product powder；
(4) (BC) is preparedxNyOzMaterial：It is the above-mentioned crude product powder of 2-6 acid elutions with pH value, is afterwards 30-80 DEG C with temperature
Deionized water is washed 1-10 times；Product after washing is dried at a temperature of 30-100 DEG C, obtained (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：It is described molten
Agent includes water, ammoniacal liquor, ethylenediamine, ethanol, ethylene glycol, acetonitrile.
3. a kind of synthesis high specific capacitance (BC) according to claim 1xNyOzThe method of material, it is characterised in that：It is described to urge
Agent includes Co, Ni, Fe.
4. a kind of high specific capacitance (BC)xNyOzMaterial, it is characterised in that：(BC)xNyOzMaterial, wherein 3≤x≤9,0.5≤y
≤ 1,0≤z≤9.
5. a kind of high specific capacitance (BC) according to claim 4xNyOzMaterial, it is characterised in that：(BC)xNyOzMaterial
Size is 1-10 μm.
6. a kind of high specific capacitance (BC) according to claim 4xNyOzMaterial, it is characterised in that：(BC)xNyOzMaterial
Specific capacitance be 400-1000F/g.
7. a kind of high specific capacitance (BC) according to claim 4xNyOzMaterial, it is characterised in that：(BC)xNyOzMaterial
For be stacked with flake, fold it is spherical or brilliant thread.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108203117A (en) * | 2017-12-25 | 2018-06-26 | 华侨大学 | A kind of TiCxNy-TiO2The synthetic method of material |
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