CN108455559A - It is a kind of based on the nitrogen boron codope porous carbon materials and its preparation method and application for breaking BN keys - Google Patents
It is a kind of based on the nitrogen boron codope porous carbon materials and its preparation method and application for breaking BN keys Download PDFInfo
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- CN108455559A CN108455559A CN201810292212.XA CN201810292212A CN108455559A CN 108455559 A CN108455559 A CN 108455559A CN 201810292212 A CN201810292212 A CN 201810292212A CN 108455559 A CN108455559 A CN 108455559A
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Abstract
The invention discloses a kind of based on the nitrogen boron codope porous carbon materials for breaking BN keys, by resorcinol, formaldehyde, hydro-thermal reaction obtains nitrogenous gel to boron nitride under alkaline condition, freeze-dried, alkali inorganic substance milled processed, carbonization, washing, dry to be made, specific surface area range is in 1000 ~ 1200 m2g‑1.Preparation method includes：1）The preparation of nitrogenous gel；2）The drying of nitrogenous gel；3）The activation of nitrogenous gel；4）The carbonization of nitrogenous gel；5）Preparation based on the porous carbon materials for breaking BN key nitrogen boron codopes.As the application of electrode material for super capacitor, current density is 20 ~ 0.5 A/g, and specific capacitance reaches 150.0 ~ 250.0 F/g.Two step doping nitrogen sources compared to the prior art and boron source, the most prominent advantage of the present invention are single step doping nitrogen source and boron source, have easily broken firm BN keys, production efficiency is greatly improved, reduces cost, has broad application prospects in ultracapacitor field.
Description
Technical field
The invention belongs to electric chemical super capacitor fields, and in particular to a kind of more based on the nitrogen boron codope for breaking BN keys
Hole carbon material.
Background technology
The increasingly shortage of sharp increase with population and economic fast development, resource and the energy becomes contemporary society urgently
One of major issue to be solved.Therefore, the exploitation of clean reproducible energy to national economic development and solves ring with application
Border problem plays crucial effect.Electric energy, wind energy, solar energy, tide energy etc. is all widely paid close attention to, and finds suitable storage
Energy device is vital link.
Ultracapacitor is a kind of novel energy storage apparatus between traditional capacitor and rechargeable battery, has power close
Degree is high, has extended cycle life, and charge-discharge velocity is fast, and use temperature range is wide, it is environmentally safe the advantages that, be applied to electronic vapour
The fields such as vehicle, aerospace and science and techniques of defence.The material of ultracapacitor is broadly divided into three kinds：Carbon material, conducting polymer
And metal oxide.Wherein, the advantages that carbon material has large specific surface area, at low cost, good conductivity.Pure carbon material surface is dredged
Water, the contact resistance for increasing electrolyte ion and hole significantly affects capacitance characteristic, and carbon material can be only formed
Electric double layer capacitance, it is nearly 100 times lower than fake capacitance, and nitrogen doped can introduce functional group in carbon material surface, can make carbon materials
Material surface wettability is improved, and electric conductivity is significantly promoted, and doping boron element can make the specific surface area and ratio of electrode material
Capacitance gets a promotion, so nitrogen boron codope porous carbon causes everybody extensive concern as electrode material.
Phenolic resin is conducted electricity very well due to cheap, and synthesis technology is easy, is had porous structure and is concerned,
Nitrogen source and boron source are introduced into phenolic resin, the electric conductivity and capacitive character of phenolic resin can be promoted.But prior art China is specially
Sharp CN201310293898.1 is disclosed, and nitrogen source and boron source will be introduced with different compounds respectively；Article《Boron and
nitrogen co-doped porous carbon with a high concentration of boron and its
superior capacitive behavior》Open, nitrogen source and boron source will not only be introduced and to be tested just by two steps respectively
Nitrogen source and boron source can be fully introduced into.
Therefore, the prior art is in the presence of due to that can not add simultaneously, preparation process caused by nitrogen and boron is complicated and the consuming time is long
The technical issues of.Therefore, how high-efficient simple while introduce nitrogen source and boron source to promote the performance of porous carbon, become vast and grind
The person's of studying carefully hot spot of interest.
Invention content
The object of the present invention is to provide a kind of based on the nitrogen boron codope porous carbon materials and preparation method thereof for breaking BN keys
And application.Nitrogen and boron element single step are mixed into phenolic resin, significantly make the synthesis procedure of nitrogen boron codope porous carbon
Easy.
Since the BN keys in boron nitride are very firm, it also is difficult to be broken even if being heated to 1000 DEG C or more.So directly
When boron nitride is mixed in phenolic resin, the BN keys in boron nitride will not be broken, and boron nitride will not be carbonized.Therefore, it is impossible to
Realize the effect of nitrogen boron codope.
The present invention, such as potassium hydroxide or sodium hydroxide, is realized under alkaline condition, in boron nitride by the way that alkaline matter is added
The fracture of BN keys, so that boron nitride is carbonized completely, nitrogen-atoms and boron atom finally can be separated into incorporation carbon material, reach nitrogen boron
The technique effect of codope porous carbon.
It is unlike the present invention and remaining nitrogen boron codope porous carbon, nitrogen and the incorporation of boron element single step is porous
Carbon improves mechanisms of electronic, has obtained high specific capacitance, inexpensive electrode material.
In order to achieve the above-mentioned object of the invention, the technical solution adopted by the present invention is：
It is a kind of based on the nitrogen boron codope porous carbon materials for breaking BN keys, by resorcinol, formaldehyde, boron nitride is under alkaline condition
After stirring at normal temperature, hydro-thermal reaction obtains nitrogen boron codope gel, freeze-dried, alkali inorganic substance activation process, and carbonization is washed
It washs, dry to be made, described nitrating porous carbon materials specific surface area ranging from 1000 ~ 1200 m2g-1。
Based on the preparation method for the nitrogen boron codope porous carbon materials for breaking BN keys, include the following steps：
Step 1）The preparation of nitrogen boron codope gel, by sodium hydroxide, resorcinol, formaldehyde, boron nitride matches in mass ratio is
0.02:1:2：（0~3）Solution stirs 3 ~ 5 hours, obtains nitrogen boron codope gel at normal temperatures；
Step 2）The drying of nitrogen boron codope gel, by nitrogen boron codope gel at subzero 40 ~ 50 DEG C, carry out freeze-drying 40 ~
50 hours, obtain dry nitrogen boron codope presoma；
Step 3）Dry nitrogen boron codope presoma and alkaline matter are 1 in mass ratio by the activation of nitrogen boron codope gel:
（1~3）Mixing is stirred 0.1 ~ 1 hour, the nitrogen boron codope presoma activated at normal temperatures, and the alkaline matter is hydrogen
Potassium oxide or sodium hydroxide；
Step 4）Nitrogen boron codope presoma after activation is put into tube furnace, in nitrogen gas by the carbonization of nitrogen boron codope gel
Under atmosphere, rises to 550 ~ 650 DEG C with 4 ~ 6 DEG C/min and 2 ~ 4 h is kept to be calcined, the nitrogen boron codope gel after being carbonized；
Step 5）Based on the preparation for the nitrogen boron codope porous carbon materials for breaking BN keys, by the nitrogen boron codope gel after carbonization,
After washing 3 ~ 5 times repeatedly with the hydrochloric acid solution of 1mol/L and deionized water, dries 10 ~ 20 hours, obtain under the conditions of 80 ~ 90 DEG C
To based on the porous carbon materials for breaking BN key nitrogen boron codopes.
Based on application of the nitrogen boron codope porous carbon materials of BN keys as electrode material for super capacitor is broken, electric current is close
Degree is 20 ~ 0.5 A/g, and specific capacitance reaches 150.0 ~ 250.0 F/g.
The present invention is through the U.S.（Quantachrome Instruments）Autosorb-1 type physical adsorption appearances, it is Dutch
Known to the test of IVIUM electrochemical workstations：The present invention is based on the nitrogen boron codope porous carbon materials specific surface areas for breaking BN keys
1000~1200 m2g-1。
The present invention is based on break application of the nitrogen boron codope porous carbon materials of BN keys as electrode material for super capacitor
When, current density is 20 ~ 0.5A/g, and specific capacitance reaches 150 ~ 250 F/g.
The present invention is based on the cyclic voltammetry test results for the nitrogen boron codope porous carbon materials for breaking BN keys to show not
Under same sweep speed, cyclic voltammetry curve keeps good and is similar to rectangular shape, has preferable electric double layer capacitance behavior
And electrochemical reversibility.
The present invention is based on the XRD spectrums for the nitrogen boron codope porous carbon materials for breaking BN keys to show that classical carbon material is bent
There is steamed bun peak respectively at 24.3 and 43.84 degree in line, it was demonstrated that has preferable degree of graphitization, and NB keys are broken, nitridation
Boron is carbonized.
The present invention is based on the XPS collection of illustrative plates for the nitrogen boron codope porous carbon materials for breaking BN keys to show C, O, N, the feature of B
Peak shows there is C, O, N in the material, and B element illustrates the successful incorporation of nitrogen and boron element.
The present invention compared with the existing technology, has the following advantages：
1, the present invention utilizes new nitrogen boron source boron nitride, makes nitrogen source and boron source that can be mixed with single step, compared to nitrogen boron before
Codoping process（It is adulterated in two steps with boric acid and nitrogen source）, high degree simplifies doping process, and is effectively mixed with
Nitrogen and boron element.
2, in aqueous electrolyte（6M KOH solutions）In, there is high specific capacitance, in 20 ~ 0.5 A/g, specific capacitance reaches
150~250 F/g。
3, the present invention, by adding alkaline matter, makes firm BN keys be beaten under alkaline condition under conditions of low temperature
It is broken, nitrogen and boron element single step are mixed into phenolic resin, significantly make nitrogen boron codope synthesis technology easy.
Therefore, the present invention is reducing synthesis technology, under conditions of taking single step doping nitrogen source and boron source, maintains electricity
The high specific capacitance of pole material, and have good high rate performance.
Description of the drawings：
Fig. 1 be the embodiment of the present invention in prepare by activation of potassium hydroxide based on the nitrogen boron codope porous carbon for breaking BN keys
The cyclic voltammetry curve of the ultracapacitor of the three-electrode system of material assembling；
Fig. 2 be the embodiment of the present invention in prepare by activation of potassium hydroxide based on the nitrogen boron codope porous carbon for breaking BN keys
Charge-discharge performance curve of the ultracapacitor of the three-electrode system of material assembling in different current densities；
Fig. 3 be the embodiment of the present invention in prepare by activation of potassium hydroxide based on the nitrogen boron codope porous carbon for breaking BN keys
The Adsorption and desorption isotherms of material；
Fig. 4 be the embodiment of the present invention in prepare by activation of potassium hydroxide based on the nitrogen boron codope porous carbon for breaking BN keys
The XRD spectrum of material；
Fig. 5 be the embodiment of the present invention in prepare without activation of potassium hydroxide based on the nitrogen boron codope porous carbon for breaking BN keys
The XRD spectrum of material；
Fig. 6 be the embodiment of the present invention in prepare by activation of potassium hydroxide based on the nitrogen boron codope porous carbon for breaking BN keys
The XPS collection of illustrative plates of material；
Specific implementation mode
The present invention is described in further detail the content of present invention by embodiment, in conjunction with Figure of description, but is not pair
The restriction of the present invention.
Embodiment
A kind of preparation method based on the nitrogen boron codope porous carbon materials for breaking BN keys：
Step 1）By sodium hydroxide, resorcinol, formaldehyde, boron nitride in mass ratio 0.02:1:2:3 mixing, weigh sodium hydroxide
0.02g, resorcinol 2.2g, formaldehyde 4.4g, boron nitride 3g are configured to solution, after being stirred 4 hours under room temperature, in 160 DEG C of conditions
Lower hydro-thermal reaction 24 hours obtains nitrogenous boron gel；
Step 2）Nitrogenous boron gel is placed under conditions of 40 degrees below zero and carries out freeze-drying 48 hours, obtains dry nitrogenous boron
Gel；
Step 3）By dry nitrogenous gel and alkali inorganic substance potassium hydroxide in mass ratio 1:2 mixing, are added appropriate distilled water,
Room temperature is ground 0.5 hour, the nitrating boron porous carbon after being activated；
Step 4）It by nitrating boron presoma, is carbonized in a nitrogen atmosphere, rises to 600 DEG C with 5 DEG C/min, kept for 3 hours, it is cold
But to room temperature, the nitrating boron porous carbon materials after being carbonized；
Step 5）Nitrogen boron codope porous carbon materials after cleaning 4 carbonizations with the hydrochloric acid solution of 1mol/L and deionized water, will
Sample is put into 85 DEG C of baking ovens, dries 12 hours, obtains based on the porous carbon materials for breaking BN key nitrogen boron codopes.
Make the fracture of BN keys to make the phenolic resin of addition boron nitride be carbonized completely to prove to be added potassium hydroxide, and
And nitrogen source and boron source has also been introduced, and it is prepared for the embodiment without activation of potassium hydroxide and is used for comparing, not specified step
It is same as the previously described embodiments, the difference is that：
The step 1）Obtain nitrogenous boron gel；
The step 2）Obtain the gel of dry nitrogenous boron；
The step 3）Unused activation of potassium hydroxide obtains the presoma of not activated nitrogenous boron；
The step 4）The porous carbon materials of nitrogenous boron after being carbonized；
The step 5）Obtain the porous carbon materials of nitrogenous boron.
Above-described embodiment prepare through activation of potassium hydroxide based on the nitrogen boron codope porous carbon materials for breaking BN keys
Cyclic voltammetry is tested, and the results are shown in Figure 1, and under different sweep speeds, cyclic voltammetry curve keeps good and is similar to
Rectangular shape has preferable electric double layer capacitance behavior and electrochemical reversibility.
Embodiment prepare through activation of potassium hydroxide based on the nitrogen boron codope porous carbon materials for breaking BN keys, test knot
For fruit as shown in Fig. 2, when current density is 0.5 A/g, specific capacitance is 237 F/g；When current density is 20 A/g, specific capacitance
Respectively 178.0 F/g have good high rate performance.
It is prepared in embodiment and tests knot based on the nitrogen boron codope porous carbon materials for breaking BN keys through activation of potassium hydroxide
Fruit is as shown in figure 3, its specific surface area is 1014 m2 g-1。
XRD spectrum such as Fig. 4 based on the nitrogen boron codope for breaking BN keys without activation of potassium hydroxide is prepared in embodiment
Shown, collection of illustrative plates is consistent with the collection of illustrative plates of boron nitride, illustrates that the structure of boron nitride is not broken.
The XRD spectrum such as Fig. 5 based on the nitrogen boron codope for breaking BN keys through activation of potassium hydroxide prepared in embodiment
It is shown, it is shown as the characteristic spectrum of carbon material, illustrates that the molecule covalent key of the boron nitride after potassium hydroxide is ground is broken,
Boron nitride is carbonized.
The XPS collection of illustrative plates such as Fig. 6 based on the nitrogen boron codope for breaking BN keys through activation of potassium hydroxide prepared in embodiment
It is shown, it can be seen that the characteristic peak of C, O, N, B illustrates to contain C in electrode material, O, N, tetra- kinds of elements of B, nitrogen and boron element
Successfully it is doped into phenolic resin.
Claims (9)
1. a kind of based on the nitrogen boron codope porous carbon materials for breaking BN keys, it is characterised in that：By resorcinol, formaldehyde, nitridation
Boron stirring at normal temperature under alkaline condition, obtains nitrogen boron codope gel after hydro-thermal reaction, freeze-dried, activate, be carbonized, washing
Wash, dry it is obtained.
2. according to claim 1 based on the nitrogen boron codope porous carbon materials for breaking BN keys, it is characterised in that：Described
Nitrating boron porous carbon materials specific surface area is 1000 ~ 1200 m2g-1。
3. a kind of preparation method based on the nitrogen boron codope porous carbon materials for breaking BN keys, it is characterised in that including following step
Suddenly：
Step 1）The preparation of nitrogen boron codope gel, by sodium hydroxide, resorcinol, formaldehyde, guanidine carbonate matched by certain mass ratio
Than being formulated as solution, stirs at normal temperatures, carrying out hydro-thermal reaction, obtaining nitrogenous boron gel；
Step 2）Nitrogen boron codope gel is freeze-dried by the drying of nitrogen boron codope gel, and it is total to obtain dry nitrogen boron
Adulterate presoma；
Step 3）Dry nitrogen boron codope presoma and alkaline matter are pressed certain mass ratio by the activation of nitrogen boron codope gel
Mixing, is activated, the nitrogen boron codope presoma activated under certain condition；
Step 4）Nitrogen boron codope presoma after activation is put into tube furnace, in certain item by the carbonization of nitrogen boron codope gel
It is calcined under part, the nitrogen boron codope gel after being carbonized；
Step 5）Based on the preparation for the nitrogen boron codope porous carbon materials for breaking BN keys, by the nitrogen boron codope gel after carbonization,
It is washed and is dried under certain condition, obtain the nitrogen boron codope porous carbon materials based on phenolic resin.
4. preparation method according to claim 3, it is characterised in that：The step 1）Sodium hydroxide, resorcinol, first
The mass ratio of aldehyde, boron nitride is 0.02:1:2：3, the step 1）The time of stirring at normal temperature is after 3 ~ 5 hours, 150 DEG C ~ 180
Hydro-thermal reaction is carried out at DEG C 20 ~ 30 hours.
5. preparation method according to claim 3, it is characterised in that：The step 2）Freeze-drying condition is freezing temperature
Degree is subzero 40 ~ 50 DEG C, and drying time is 40 ~ 50 hours.
6. preparation method according to claim 3, it is characterised in that：The step 3）Nitrogen boron codope presoma：Hydrogen-oxygen
The mass ratio for changing potassium is 1:（1~3）, the step 3）The condition of activation is to grind 0.1 ~ 1 hour at normal temperatures, the step 3）
Alkaline matter be potassium hydroxide or sodium hydroxide.
7. preparation method according to claim 3, it is characterised in that：The step 4）The condition of carbonization is nitrogen atmosphere
Under, it rises to 550 ~ 650 DEG C with 4 ~ 6 DEG C/min and 2 ~ 4 h is kept to be calcined.
8. preparation method according to claim 3, it is characterised in that：The step 5）Washing and dry condition are to use
After the hydrochloric acid solution of 1mol/L washs 3 ~ 5 times repeatedly with deionized water, dried 10 ~ 20 hours under the conditions of 80 ~ 90 DEG C.
9. it is a kind of based on breaking application of the nitrogen boron codope porous carbon materials of BN keys as electrode material for super capacitor, it is special
Sign is：Current density is 20 ~ 0.5 A/g, and specific capacitance reaches 150.0 ~ 250.0 F/g.
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