CN104760944B - One one step preparation method of double-face isomeric net carbon film - Google Patents
One one step preparation method of double-face isomeric net carbon film Download PDFInfo
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Abstract
The present invention relates to an one step preparation method of a kind of double-face isomeric net carbon film, under conditions of being passed through noble gas, composite membrane two-sided to PVDF/PET carry out pre-carbonization, activate, recarbonize after obtain double-face isomeric net carbon film.Compared with prior art, the present invention, using the two-sided composite membrane of PVDF/PET as the predecessor of reaction, itself intrinsic net carbon structure, adds carbonization, and activation improves the specific surface area of porous carbon materials.The present invention has synthesized one-step method double-face isomeric net carbon film first by calcination method, and the technique of the present invention is simple, and preparation condition is general; product morphology is stable, purity is high; and product processes convenient succinct, it is not necessary to take loaded down with trivial details protective measure, experimental facilities and condition are required low.Double-face isomeric net carbon film prepared by the present invention is a kind of low price, good conductivity, specific surface area is big, hole is flourishing material, has good electrochemical properties and the potentiality as ultracapacitor in theory.
Description
Technical field
The present invention relates to an one step preparation method of double-face isomeric net carbon film, belong to technical field of inorganic nanometer material.
Background technology
Material with carbon element, owing to having fabulous electric conductivity and big specific surface area, particularly porous carbon materials, is a kind of
Extraordinary super capacitor material.Common porous carbon materials structure comparison is single, and performance is also the most single, compares it
Under, the net carbon film of such double-face isomeric can have two kinds of different structures on same film, structures shape character,
The character thus drawn is each variant.If modifying material of the same race on two sides, then the structure on two sides the most just differs
Sample, if modifying different materials according to different needs, then have various function.
Pvdf membrane i.e. polyvinylidene fluoride film (polyvinylidene fluoride) is conventional in western blotting
A kind of solid support.Pvdf membrane is hydrophobic, and membrane aperture varies.Kynoar, as high score
A member of son, has the best mechanical performance, and the HF produced during its pyrolysis can expand pore-size distribution, from
And improve the specific surface area of material with carbon element.PET is commonly called as polyester resin, and it is the condensation polymer of p-phthalic acid and ethylene glycol.
Its mechanical property is good, heat-resisting, nontoxic, tasteless, and wholesomeness is good.The film two sides prepared by both materials
Structure is different, and the porous carbon materials obtained after carbonization is also different.Basis based on commercial membranes
The net carbon structure that body is intrinsic, adds carbonization, and activation improves the specific surface area of porous carbon materials.
In document, synthesizing porous material with carbon element mainly prepares porous carbon materials with biological material carbonization at present.Porous is multiple
Close material with carbon element primary synthetic methods and have the method such as activation method, masterplate method.And conventional porous carbon materials does not exist two-sided
The characteristic of isomery, does not possess the ultracapacitor character of excellence.
Summary of the invention
The purpose of the present invention is just directed to improve the shortcoming that porous carbon materials structure is single, pore-size distribution is narrow, and
One one step preparation method of a kind of double-face isomeric net carbon film is provided.The inventive method improves ratio electric capacity and the knot of material
Structure multiformity, thus certain place mat should be used as it in ultracapacitor field.By conductive porous material with carbon element
With being combined of metal, integrate both superioritys, reach to improve the target of super capacitor material performance.
The purpose of the present invention can be achieved through the following technical solutions:
An a kind of one step preparation method of double-face isomeric net carbon film, under conditions of being passed through noble gas, right
The two-sided composite membrane of PVDF/PET carry out pre-carbonization, activate, recarbonize after obtain double-face isomeric net carbon film.
Specifically include following steps:
(1) composite membrane two-sided to PVDF/PET carries out pre-carbonization:
Two-sided for PVDF/PET composite membrane is put in porcelain boat, then porcelain boat is put into tube furnace, lazy being passed through
Property gas under conditions of, be gradually heating to preheat temperature, the pre-heat treatment, make the two-sided composite membrane of PVDF/PET
Porous network structure settles out, and obtains pre-carbonized samples；
(2) activation processing:
The pre-carbonized samples of step (1) gained is naturally cooled under room temperature, with NaOH, pre-carbonized samples is carried out
Activation, obtains sample after activation；
(3) process is recarbonized:
Step (2) gained sample after activation is put in tube furnace, under conditions of being passed through noble gas, gradually
It is warming up to carburizing temperature, under carburizing temperature, is incubated 2h it is carried out carbonization, obtain double-face isomeric net carbon film, move back
It is cooled to room temperature after fire, sample is washed, be centrifuged, be dried, collect and obtain double-face isomeric net carbon film.
Preferably, described noble gas is argon or nitrogen.
Preferably, step (1) carries out in pre-carbonization, and described preheating temperature is 300-450 DEG C.
Preferably, step (1) carries out, in pre-carbonization, being warming up to 150-200 DEG C with 1-5 DEG C/min, and insulation 1 is little
Shi Hou, after being warming up to preheat temperature with 1-2 DEG C/min, is incubated two hours.
Preferably, in the activation processing described in step (2), NaOH is 3:1 with the mass ratio of pre-carbonized samples.
Preferably, recarbonize in process described in step (3), be warming up to carburizing temperature with 5 DEG C/min, described
Carburizing temperature be 700-800 DEG C.
In a preferred embodiment, after step (1) completes pre-carbonization treatment, to pre-carbonized samples nitre
Acid ferrous solution impregnate at normal temperatures, be then sonicated and make pre-carbonized samples mix homogeneously with ferric nitrate, be then dried to
Powder, carries out activation processing described in (2) afterwards and recarbonizes process described in step (3), being loaded
The double-face isomeric net carbon film of ferrum.
Preferably, described pre-carbonized samples is 1:1 with the weight ratio of ferric nitrate.
The two-sided composite membrane of described PVDF/PET is a kind of commercially available product film, it is also possible to use is discarded
The two-sided composite membrane of PVDF/PET, it is achieved the recycling of refuse.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1), in the present invention, using the two-sided composite membrane of PVDF/PET as the predecessor of reaction, PVDF/PET is double
Face composite membrane is a kind of commercial membranes with two-sided unlike material and structure, and composite membrane two-sided to PVDF/PET enters
Row differential thermal analysis is tested, and obtains the thermal property of the two-sided composite membrane of PVDF/PET, two-sided multiple according to PVDF/PET
Close film TG figure and DSC figure can be seen that this kind of two-sided composite membrane has Mass lost at 150 DEG C, material has been described
Decomposing, this explanation PVDF can decompose at this temperature, additionally has a peak upwards at 250 DEG C, belongs to
The endothermic reaction, this is that PET decomposes in atmosphere.The melt temperature that can be seen that this two-sided composite membrane is 120 DEG C,
Glass transition temperature is 200 DEG C, and the most this composite membrane is adapted for calcining.Raw material is simple and easy to get, low cost
Honest and clean.
(2) it is a kind of commercial membranes due to the two-sided composite membrane of PVDF/PET, itself intrinsic net carbon structure, then add
Upper carbonization, activation improves the specific surface area of porous carbon materials.
(3) present invention achieves and utilize common commercial film for presoma, synthesized one-step method by calcination method first
Double-face isomeric net carbon film, the technique of the present invention is simple, and preparation condition is general, and product morphology is stable, purity is high, and
Product processes convenient succinct, it is not necessary to take loaded down with trivial details protective measure, requires low to experimental facilities and condition.
(4) method of the present invention has higher control to the pattern of product.Controlled by the heating rate of calcining
Product morphology processed, still further aspect is that last aspect is exactly carbonization time, the present invention by setting carburizing temperature
In, heating rate is set to 1 DEG C per minute, and carburizing temperature is set as 800 DEG C, sets carbonization time as 2h, right
Product keeps pattern optimal.
(5) product prepared by the present invention is with a wide range of applications, and can apply to electro-catalysis, super capacitor
Device, energy storage, the aspect such as energy battery, potential for solving energy problem.
(6) the double-face isomeric net carbon film that prepared by the present invention be a kind of low price, good conductivity, specific surface area greatly, hole
The material that gap is flourishing, it is theoretical that these characteristics just provide some to this material as ultracapacitor and electrode material
Basis.The hole of double-face isomeric net carbon film prepared by the present invention is flourishing, has graded porous structure, the most permissible
Realize the biggest specific surface area, add this characteristic of double-face isomeric and just can load different materials or same
Material different-shape, can select the load waken up thus give its particularity function, so make the fortune of this material
With more extensive, unique.There are good electrochemical properties and the potentiality as ultracapacitor the most in theory.
Accompanying drawing explanation
Fig. 1 is embodiment 1 gained double-face isomeric net carbon film one side Electronic Speculum figure under the multiple of 3um；
Fig. 2 is embodiment 1 gained double-face isomeric net carbon film another side Electronic Speculum figure under the multiple of 5um；
Fig. 3 is the N of embodiment 1 gained double-face isomeric net carbon film2De--adsorption curve；
Fig. 4 is the graph of pore diameter distribution of embodiment 1 gained double-face isomeric net carbon film；
Fig. 5 is embodiment 2 gained double-face isomeric net carbon film one side Electronic Speculum figure under the multiple of 500nm；
Fig. 6 is embodiment 2 gained double-face isomeric net carbon film one side Electronic Speculum figure under the multiple of 2um；
Fig. 7 is embodiment 2 gained double-face isomeric net carbon film another side Electronic Speculum figure under the multiple of 5um；
Fig. 8 is the XRD figure spectrogram of embodiment 2 gained double-face isomeric net carbon film；
Fig. 9 is the Raman spectrogram of embodiment 2 gained double-face isomeric net carbon film；
Figure 10 is the N of embodiment 2 gained double-face isomeric net carbon film2De--adsorption curve；
Figure 11 is the graph of pore diameter distribution of embodiment 2 gained double-face isomeric net carbon film；
Figure 12 is the XRD figure spectrogram of embodiment 3 gained double-face isomeric net carbon film.
Detailed description of the invention
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
One one step preparation method of a kind of double-face isomeric net carbon film, under conditions of being passed through nitrogen, to PVDF/PET
Two-sided composite membrane carries out pre-carbonization, recarbonize after obtain double-face isomeric net carbon film.Specifically include following steps:
(1) composite membrane two-sided to PVDF/PET carries out pre-carbonization:
Two-sided for PVDF/PET composite membrane is put in porcelain boat, then porcelain boat is put into tube furnace, be passed through nitrogen
Under conditions of gas, it is warming up to 150 DEG C with 5 DEG C/min, is incubated 1 hour, then is warming up to 300 DEG C with 1 DEG C/min,
It is incubated two hours, carries out the pre-heat treatment, make the porous network structure of the two-sided composite membrane of PVDF/PET settle out,
Obtain pre-carbonized samples；
(2) process is recarbonized:
Step (1) gained sample is put in tube furnace, under conditions of being passed through nitrogen, heats up with 5 DEG C/min
To 700 DEG C, it is incubated and it was carried out carbonization in 2 hours, obtain double-face isomeric net carbon film, after annealing, be cooled to room
Temperature, washs sample, is centrifuged, is dried, collect and obtain double-face isomeric net carbon film.
The two-sided composite membrane of PVDF/PET that the present embodiment is used is a kind of commercially available product film, chooses in Shanghai
Rank Chemical Industry Science Co., Ltd.
The Electronic Speculum figure of the double-face isomeric net carbon film that the present embodiment obtains as shown in Figure 1 and Figure 2, it will be seen from figure 1 that
The product obtained wherein one side has the structure of porous, and pore-size distribution ratio is wide, and maximum diameter is about 0.3 μ
M, little up to 0.01 μm, from figure, can be seen that void ratio is more flourishing；Products obtained therefrom as can be seen from Figure 2
The Electronic Speculum figure of another side, can be seen that from Fig. 2 and has the material of lamellar to load on this net carbon film, diameter
It is about 2 microns, stands upright on as petal above net carbon film, which increase the specific surface area of this kind of product.
The N of the double-face isomeric net carbon film that the present embodiment obtains2De--adsorption curve is as shown in Figure 3, it can be seen that gained
The specific surface area of product and adsorpting type, can be seen that from Fig. 3 the double-face isomeric net carbon film that the present embodiment obtains belongs to
Taking off-absorption in type Ι with H4 hysteresis curve, specific surface area is up to 689.26m2g-1.Graph of pore diameter distribution is such as
Shown in Fig. 4, void content is up to 1.13cm as can be seen from Figure 43g-1。
Embodiment 2
One one step preparation method of a kind of double-face isomeric net carbon film, under conditions of being passed through nitrogen, to PVDF/PET
Two-sided composite membrane carry out pre-carbonization, activate, recarbonize after obtain double-face isomeric net carbon film.Specifically include following steps:
(1) composite membrane two-sided to PVDF/PET carries out pre-carbonization:
Two-sided for PVDF/PET composite membrane is put in porcelain boat, then porcelain boat is put into tube furnace, be passed through nitrogen
Under conditions of gas, it is warming up to 200 DEG C with 1 DEG C/min, is incubated 1 hour, then is warming up to 450 DEG C with 2 DEG C/min,
It is incubated two hours, carries out the pre-heat treatment, make the porous network structure of the two-sided composite membrane of PVDF/PET settle out,
Obtain pre-carbonized samples；
(2) activation processing:
The pre-carbonized samples of step (1) gained is naturally cooled under room temperature, with NaOH, pre-carbonized samples is carried out
Activation, NaOH is 3:1 with the mass ratio of pre-carbonized samples, obtains sample after activation；
(3) process is recarbonized:
Step (2) gained sample after activation is put in tube furnace, under conditions of being passed through nitrogen, with 5 DEG C/min
It is warming up to 800 DEG C, is incubated two hours, it is carried out carbonization, obtain double-face isomeric net carbon film, cold after annealing
But to room temperature, sample is washed, be centrifuged, be dried, collect and obtain double-face isomeric net carbon film.
The two-sided composite membrane of PVDF/PET that the present embodiment is used is a kind of commercially available product film, chooses in Shanghai
Rank Chemical Industry Science Co., Ltd.
The Electronic Speculum figure of the double-face isomeric net carbon film that the present embodiment obtains is as shown in Fig. 5～Fig. 7, and Fig. 5-Fig. 7 is not
Scheming with the SEM under up-sizing, SEM figure can be seen that have 100nm size on obtained net carbon film
Hole, belongs to porous material in one, and structure is like cellular, and what Fig. 7 represented is the another of double-face isomeric net carbon film
The structure of outer one side, is also a kind of loose structure, and pore-size distribution is extensive, aperture substantially 0.1 μm-5 μm, this
The pore-size distribution of sample is conducive to increasing its specific surface area, thus more preferably applies in ultracapacitor.
As shown in Figure 8, the XRD of Fig. 8 is clear and definite for the XRD spectrum of the double-face isomeric net carbon film that the present embodiment obtains
This material that indicates there are typical 24.3 ° of Graphene peaks, such structure can strengthen and change material
Electrochemical properties.Here there are two characteristic peaks, about 1344.11cm-1And 1586.21cm-1, such feature
Peak can be produced by band by D and G, can be seen that the Graphene having reached certain from figure, is more beneficial for using
In electrode material.
The Raman spectrogram of the double-face isomeric net carbon film that the present embodiment obtains is as it is shown in figure 9, there are two features here
Peak, about 1344.11cm-1And 1586.21cm-1, such characteristic peak can be produced by band by D and G,
From figure, can be seen that the Graphene having reached certain, be more beneficial for for electrode material.Figure 10 shows two-sided
Suction-the desorption of heterogeneous network carbon film belongs to type Ι, and specific surface area can up to 1296m2g-1.Figure 11 represents this material
Pore-size distribution extensive, macropore, mesoporous, aperture has, and void content can reach 1.33cm3g-1, aperture model
It is trapped among 1-10nm.
Embodiment 3
One one step preparation method of a kind of double-face isomeric net carbon film, under conditions of being passed through argon, to PVDF/PET
Two-sided composite membrane carry out pre-carbonization, activate, recarbonize after obtain double-face isomeric net carbon film.Specifically include following steps:
(1) composite membrane two-sided to PVDF/PET carries out pre-carbonization:
Two-sided for PVDF/PET composite membrane is put in porcelain boat, then porcelain boat is put into tube furnace, be passed through argon
Under conditions of gas, it is warming up to 200 DEG C with 1 DEG C/min, is incubated 1 hour, then is warming up to 450 DEG C with 2 DEG C/min,
It is incubated two hours, the pre-heat treatment, make the porous network structure of the two-sided composite membrane of PVDF/PET settle out,
To pre-carbonized samples；
(2) the pre-carbonized samples iron nitrate solution of 1% (mass fraction) is impregnated 12 hours at normal temperatures,
Wherein, the weight ratio of pre-carbonized samples and ferric nitrate is 1:1, is then sonicated 30 minutes, make pre-carbonized samples with
Ferric nitrate mix homogeneously, is then dried to powder；
(3) activation processing:
It is activated by step (2) gained powdered samples NaOH, NaOH and pre-carbonized samples
Mass ratio is 3:1, obtains sample after activation；
(4) process is recarbonized:
Step (3) gained sample after activation is put in tube furnace, under conditions of being passed through argon, with 5 DEG C/min
It is warming up to 800 DEG C, is incubated two hours, it is carried out carbonization, obtain double-face isomeric net carbon film, cold after annealing
But to room temperature, sample is washed, be centrifuged, be dried, collect and obtain double-face isomeric net carbon film.
The two-sided composite membrane of PVDF/PET that the present embodiment is used is a kind of commercially available product film, chooses in Shanghai
Rank Chemical Industry Science Co., Ltd.
As shown in figure 12, Figure 12 illustrates this material to the XRD spectrum of the double-face isomeric net carbon film that the present embodiment obtains
Being a kind of amorphous carbon material, be a kind of graphene-structured, on picture, 200,210, the 310 of display represent respectively
Fe, Fe has been loaded on this material3O4、Fe2O3。
The above-mentioned description to embodiment is to be understood that for ease of those skilled in the art and use to send out
Bright.These embodiments obviously easily can be made various amendment by person skilled in the art, and at this
The General Principle illustrated is applied in other embodiments without through performing creative labour.Therefore, the present invention does not limits
In above-described embodiment, those skilled in the art are according to the announcement of the present invention, without departing from changing that scope is made
Entering and revise all should be within protection scope of the present invention.
Claims (6)
1. an one step preparation method of a double-face isomeric net carbon film, it is characterised in that be passed through the bar of noble gas
Under part, composite membrane two-sided to PVDF/PET carry out pre-carbonization, activate, recarbonize after obtain double-face isomeric net carbon
Film, specifically includes following steps:
(1) composite membrane two-sided to PVDF/PET carries out pre-carbonization:
Two-sided for PVDF/PET composite membrane is put in porcelain boat, then porcelain boat is put into tube furnace, lazy being passed through
Property gas under conditions of, be gradually heating to preheat temperature, the pre-heat treatment, described preheating temperature is 300-450 DEG C,
The porous network structure making the two-sided composite membrane of PVDF/PET settles out, and obtains pre-carbonized samples；
(2) activation processing:
The pre-carbonized samples of step (1) gained is naturally cooled under room temperature, with NaOH, pre-carbonized samples is carried out
Activation, NaOH is 3:1 with the mass ratio of pre-carbonized samples, obtains sample after activation；
(3) process is recarbonized:
Step (2) gained sample after activation is put in tube furnace, under conditions of being passed through noble gas, with 5 DEG C
/ min is warming up to carburizing temperature, and described carburizing temperature is 700-800 DEG C, is incubated 2h to it under carburizing temperature
Carry out carbonization, obtain double-face isomeric net carbon film, after annealing, be cooled to room temperature, sample is washed, be centrifuged,
It is dried, collects and obtain double-face isomeric net carbon film.
One one step preparation method of a kind of double-face isomeric net carbon film the most according to claim 1, it is characterised in that
Described noble gas is argon or nitrogen.
One one step preparation method of a kind of double-face isomeric net carbon film the most according to claim 1, it is characterised in that
Step (1) carries out, in pre-carbonization, being warming up to 150-200 DEG C with 1-5 DEG C/min, after being incubated 1 hour, with 1-2 DEG C
After/min is warming up to preheat temperature, it is incubated two hours.
One one step preparation method of a kind of double-face isomeric net carbon film the most according to claim 1, it is characterised in that
After step (1) completes pre-carbonization treatment, pre-carbonized samples iron nitrate solution is impregnated at normal temperatures, then surpasses
Sonication makes pre-carbonized samples mix homogeneously with ferric nitrate, is then dried to powder, carries out afterwards described in (2)
Activation processing and step (3) described in recarbonize process, obtain the double-face isomeric net carbon film of load iron.
One one step preparation method of a kind of double-face isomeric net carbon film the most according to claim 4, it is characterised in that
Described pre-carbonized samples is 1:1 with the weight ratio of ferric nitrate.
One one step preparation method of a kind of double-face isomeric net carbon film the most according to claim 1, it is characterised in that
The two-sided composite membrane of described PVDF/PET is a kind of commercially available product film.
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| CN1830533A (en) * | 2005-12-13 | 2006-09-13 | 大连理工大学 | Preparation method of polyether sulphone ketone base gas separation carbon membrane |
| CN101979316A (en) * | 2010-11-02 | 2011-02-23 | 上海大学 | Method for preparing active carbon material by using waste and old polyethylene glycol terephthalate |
| CN102800489A (en) * | 2012-08-07 | 2012-11-28 | 中国人民解放军63971部队 | Preparation method of carbon electrode material with gradation pore structure for supercapacitor |
| CN103121678A (en) * | 2012-12-14 | 2013-05-29 | 大连理工大学 | Method for preparing nitrogen-doped activated carbon by utilizing PET (polyethylene terephthalate) waste material |
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|---|---|---|---|---|
| CN1830533A (en) * | 2005-12-13 | 2006-09-13 | 大连理工大学 | Preparation method of polyether sulphone ketone base gas separation carbon membrane |
| CN101979316A (en) * | 2010-11-02 | 2011-02-23 | 上海大学 | Method for preparing active carbon material by using waste and old polyethylene glycol terephthalate |
| CN102800489A (en) * | 2012-08-07 | 2012-11-28 | 中国人民解放军63971部队 | Preparation method of carbon electrode material with gradation pore structure for supercapacitor |
| CN103121678A (en) * | 2012-12-14 | 2013-05-29 | 大连理工大学 | Method for preparing nitrogen-doped activated carbon by utilizing PET (polyethylene terephthalate) waste material |
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