CN105000553B - A kind of method that thermo-contact formula prepares nano aperture Graphene - Google Patents
A kind of method that thermo-contact formula prepares nano aperture Graphene Download PDFInfo
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Abstract
The invention discloses a kind of method that thermo-contact formula prepares nano aperture Graphene, it is characterised in that：By the dry graphite oxide ene product such as graphite oxide aerogel or graphene oxide paper, Direct Contact Heating thermal source spontaneous combustion expansion reduction is obtained under relatively lower temp.The present invention is by the use of the dry graphite oxide ene product such as graphite oxide aerogel as the material for preparing Graphene, and Direct Contact Heating thermal source in air atmosphere, there is spontaneous combustion within of short duration several seconds and expand, most of oxygen-containing functional group is rapidly sloughed in gaseous form simultaneously, and hole is produced in fault location, such that it is able to extensive and rapidly and efficiently the Graphene for preparing bigger serface, nano aperture.
Description
Technical field
The present invention relates to the preparation method of nano aperture Graphene.
Technical background
Graphene, a two-dimentional carbon material for atomic thickness, due to the specific surface area (~2630m of its superelevation2/ g), it is considerable
Thermal conductivity, excellent electrical conductivity and mechanical performance, it is continual in the past few years to attract much attention.It is unique
Structure and excellent performance make Graphene in the field of electronic device, sensor and energy stores/conversion etc. have more
It is widely applied.However, Graphene would generally occur irreversible stacking during preparation and use, due to its interlayer compared with
The interaction of strong pi-pi bond and van der waals force forms graphite linings, causes specific surface area to strongly reduce.When it is using super
When level electrode for capacitors, lithium battery etc. are middle, it is unfavorable for that electrolyte is preferably transmitted, have impact on the expression of chemical property.
In order to make full use of Graphene high-specific surface area inherently, people start for notice to be transferred to hole graphite
In the research of alkene, wherein comprising nanometer grid Graphene, fold Graphene, foamy graphite alkene；Due to its special loose structure,
Specific surface area high and pore volume high, and Graphene property inherently is combined, hole Graphene turns into people for the moment
The focus of research.It is worth noting that, hole Graphene separates/storage in electronics and photovoltaic device, energy storage, gas,
The field such as absorption oil and sensor has obtained relatively broad application.
In recent years, people attempt preparing hole Graphene with different modes, wherein photoengraving, electronics etching and wait from
Daughter etching can obtain the homogeneous Graphene of hole, but these preparation methods can not be mass produced, and limited it and used model
Enclose.Someone obtains the Graphene of nano aperture using KOH etching oxidation Graphenes, but preparation process introduces KOH, also to remove
KOH, total preparation flow not only expends the time, can also produce more mass loss.Other preparation methods, such as organic molecule
Synthesis, template, Hydrothermal Synthesiss, electronation and template direction CVD etc., part way introduces some acid-base reagents, gold
Category oxide utilizes the conditions such as special etching, sealing, high pressure, high temperature, template, on the one hand not environmentally, on the other hand makes
It is higher for the hole Graphene cost for going out, it is unsuitable for large-scale preparation.Recently, the mode of someone's thermal expansion prepares many
Hole Graphene, but they use graphene oxide powder or the dry graphene oxide solid of bulk to prepare, system
Standby process produces stronger volumetric expansion, causes powder to waft, not easily collecting, and not safe enough.
The content of the invention
The present invention is to avoid the weak point existing for above-mentioned preparation method, there is provided a kind of simple and environmentally-friendly and suitable big
The preparation method of the nano aperture Graphene of large-scale production.
The present invention is adopted the following technical scheme that to solve technical problem：
The method that thermo-contact formula of the present invention prepares nano aperture Graphene, its feature is：
Carry out as follows：
Step a, by graphene oxide dispersion in deionized water, obtain graphene oxide suspension；
Step b, freeze-drying is carried out to graphene oxide suspension, obtain graphite oxide aerogel；Or to oxidation stone
Black alkene suspension carries out freeze-day with constant temperature, obtains graphene oxide paper；
Step c, in air atmosphere, by heat source be preheated to 200 DEG C and more than, after stabilizing the temperature, by the oxygen
Graphite alkene aeroge is placed on heat source, makes graphite oxide aerogel burning expansion, and graphene oxide is reduced, that is, obtain
Obtain nano aperture graphene aerogel；Or in air atmosphere, by heat source be preheated to 200 DEG C and more than, in temperature stabilization
Afterwards, the graphene oxide paper is placed on heat source, makes graphene oxide paper burning expansion, graphene oxide is reduced,
Obtain nano aperture graphene paper.
Preferably, the concentration of graphene oxide suspension described in step a is 4~10mg/mL.If concentration is too low, can cause
Prepare the tight ness rating of sample of graphite oxide aerogel and graphene oxide paper not enough, and produce substantial amounts of sample loss；It is dense
Spend height be unfavorable for the dispersion of graphene oxide, and can cause thermo-contact process result in, the sample specific surface area for obtaining
There is certain loss.
Freeze-drying described in step b is carried out under conditions of -40 DEG C~-60 DEG C.
Freeze-day with constant temperature described in step b is carried out under conditions of 55 DEG C~65 DEG C.
Heat source described in step c can be any one in warm table, tube furnace, electric hot plate or electromagnetic oven, or
Other instruments that can arbitrarily heat in atmosphere.
The preheating temperature of heat source is preferably 200~300 DEG C described in step c, and this temperature range can meet instead
Answer and can produce identical effect under demand, high-temperature condition, so without temperature higher.At 200 DEG C, by graphene oxide gas
Gel or graphene oxide paper are placed on heat source, have the preheating of 2~5s, and then rapid burning exists since its contact point
Whole graphite oxide aerogel or graphene oxide paper, whole combustion process only need 0.01s or so, that is, complete burning, reaction
Rapidly.At 300 DEG C, graphite oxide aerogel or graphene oxide paper are placed on heat source need not be preheated substantially,
Directly just rapid burning is complete since contact point, and whole combustion process also only needs 0.01s.
The nano aperture model of nano aperture graphene aerogel or nano aperture graphene paper as obtained by the inventive method
It is trapped among between 1.5nm-100nm, both contains micropore, also contains mesoporous and macropore；Specific surface area is in 280-1000m2Between/g.
In the present invention, in the preparation process of graphene oxide, because strong oxidation introduces substantial amounts of defect
And oxygen-containing functional group.By freeze-drying or freeze-day with constant temperature, after being prepared into graphite oxide aerogel or graphene oxide paper, do
Dry graphite oxide aerogel or graphene oxide paper contact thermal source, the carbon of defective locations reaches ignition point generation at contact point
Spontaneous combustion, the nano aperture of a part is produced in burning point, while producing substantial amounts of heat, makes oxygen-containing functional group in gaseous form
(CO2, O2, CO, H2O) slough rapidly, larger interlayer air pressure is produced, more than interlayer van der waals force so that splitting
And expand, escaping gas gets nano aperture in the poor position of Graphene crystal property in addition.The heat offer that burning is produced
To adjacent graphene oxide, it is burnt and produce identical experiment effect.Whole combustion process is no more than 0.01s.
Compared with the prior art, the present invention has the beneficial effect that：
1st, the present invention obtains graphene oxide gas by by the drying of graphene oxide suspension directly freezed or freeze-day with constant temperature
Gel or graphene oxide paper as experiment original material, it is to avoid using graphene oxide powder material strips come powder float
Fly problem；It also avoid the dangerous and collection inconvenience brought using the heating expansion of dry graphene oxide bulk solid, green,
Environmental protection, safety.
2nd, the present invention utilizes warm table at relatively low temperature (>=200 DEG C), and in air atmosphere, directly contact adds
Thermal source redox graphene, it is not necessary to the condition of special sealing, vacuum, gas treatment and HTHP.
3rd, the present invention is in operation without the addition of any pollutant, environmental protection, quick and convenient.
4th, preparation method of the invention can on a large scale and rapidly and efficiently bigger serface processed, nano aperture reduction-oxidation graphite
Alkene, its cost performance is higher, and gained graphite nanometer hole scope is interval in 1.5nm-100nm, both contains micropore, also containing mesoporous
And macropore.Its specific surface area is in 280-1000m2Between/g；And can be utilized in ultracapacitor, lithium ion battery, conduction
The various fields such as filler.
Brief description of the drawings
In Fig. 1,1-a is the filemot graphite oxide aerogel prepared by embodiment 1；1-b is prepared by embodiment 1
Black nano aperture graphene aerogel；
In Fig. 2,2-a, 2-b are respectively graphite oxide aerogel (GO) and the nano aperture graphite prepared by embodiment 1
The XPS collection of illustrative plates of alkene aeroge (300-RGO).
In Fig. 3,3-a is that the electrochemistry cyclic voltammetric of the nano aperture Graphene (300-RGO) prepared by embodiment 1 is bent
Line；3-b is the constant temperature current charge-discharge electricity curve of Graphene；3-c is that the specific capacitance value of 12000 cycle charge-discharges of Graphene is followed
Ring stability figure.
In Fig. 4, the material for preparing is done in Raman analysis testing example 1, solid line is graphene oxide (i.e. GO), and dotted line is
300 DEG C of heat treatments reduce the Raman figures of the Graphene (RGO) for obtaining.
In Fig. 5, prepared hole Graphene, Fig. 5-a, 5-b point in transmission electron microscope (TEM) sign embodiment 1
It is not that scale is the transmission electron microscope picture under 50nm and 20nm.
In Fig. 6,6-a and 6-b is respectively the specific surface area test chart of the hole Graphene obtained in embodiment 1 and corresponding
Pore analysis figure.
In Fig. 7,7-a is the smooth graphene oxide paper (GO) in filemot surface in embodiment 2, and 7-b is swollen black
Swollen shaggy nano aperture graphene paper (RGO).7-c, 7-d are respectively graphene oxide (GO) and nano aperture graphite
Optical photograph of the cross section of alkene (RGO) under 50 times of enlargement ratios of light microscope.
In Fig. 8,8-a and 8-b is the specific surface area test chart of the nano aperture Graphene prepared in embodiment 2 and corresponding
Pore analysis figure.
In Fig. 9,9-a and 9-b be respectively the brown before being heat-treated in embodiment 3 graphite oxide aerogel and
The optical photograph of the hole Graphene of the black after 200 DEG C of warm table treatment.
In Figure 10,10-a and 10-b is respectively the specific surface area test chart and phase of the hole Graphene obtained in embodiment 3
The pore analysis figure answered.
Specific embodiment
Embodiment 1
The present embodiment graphite oxide aerogel prepares bigger serface, nano aperture Graphene airsetting as raw material
Glue, is carried out in accordance with the following steps：
Step a, graphene oxide being prepared with improving Hummers methods, and being separated into suspension with deionized water, concentration is
10mg/mL。
Step b, by the graphene oxide suspension freeze-drying in step a：Graphene oxide suspension is first placed on ice
Solid is frozen into case, is placed into during cold well temperature has reached -50 DEG C of freeze drier and is dried, you can obtain graphene oxide gas
Gel, the brown column aeroge solid as shown in Fig. 1-a.
Under step c, air atmosphere, warm table is preheated, temperature adjustment to 300 DEG C, after after temperature stabilization, by step b
In graphite oxide aerogel be directly placed on warm table.Wait about 0.1 second, graphite oxide aerogel adds from contact
The contact point of thermal station starts burning, to the burning of whole aeroge totally, burn time duration about 0.01s.Can obtain as shown in Fig. 1-b
Black nano aperture graphene aerogel.TEM figures in Fig. 5-a and 5-b clearly can be found out on graphene film
Nano aperture, about 1-5nm.
The graphite oxide aerogel obtained in step b and step c and the nano aperture graphene aerogel for obtaining are done
XPS analysis, as shown in Figure 2,2-a, 2-b are respectively the XPS of graphite oxide aerogel and nano aperture graphene aerogel
Collection of illustrative plates, the oxygen-containing functional group peak value reduction of the redox graphene after being as can be seen from the figure heat-treated is a lot, that is, aoxidize stone
Black alkene major part oxygen-containing functional group is removed.
Electro-chemical test is done, the nano aperture graphene aerogel that will be obtained in step c is prepared into electrode：By Graphene,
Kynoar and acetylene black in mass ratio 40:5:5 it is well mixed after add N methyl pyrrolidone (NMP) reagent, stir into mud
Bar shape, be applied on nickel foam collector, 60 DEG C insulating boxs dry.With the KOH solution of 6mol/L as electrolyte,
, used as to electrode, used as reference electrode, the electrode of preparation is used as working electrode for Ag/AgCl electrodes for Pt electrodes.Respectively 0.01,
0.05th, 0.10 volt-ampere curve, is tested under the scanning voltage speed of 0.20V/s, as shown in Fig. 3-a, it can be seen that with scanning speed
The increase of rate, the area that curve is surrounded also gradually increases, and the shape of curve shows preferable electric double layer capacitance close to rectangle
Energy.Permanent steady current charge-discharge electrical testing is done under the current density of 0.1A/g, as shown in Fig. 3-b, by formula Cg=(I Δs t)/
(m Δ V) calculates specific capacitance for 244.73F/g.Wherein Cg is specific capacitance；I is charging and discharging currents density；T is discharge time；
M is active material quality on working electrode；V is potential window.Specific capacitance unit is F/g.
The test of cyclical stability, as shown in Fig. 3-c, under permanent steady current charge-discharge power mode, with the discharge and recharge electricity of 10A/g
Current density cycle charge-discharge 12000 times, using above mentioned specific capacitance computing formula, calculates the ratio electricity of every 500 circulations
Hold, make data needed for figure.By 12000 cycle charge-discharges, specific capacitance remains in that more than the 96.8% of initial value,
The nano aperture Graphene that this is obtained has preferable cyclical stability in the utilization of ultracapacitor.
Raman is tested, and the graphene oxide and hole Graphene that are prepared in step b and step c are done into Raman test respectively,
As shown in Figure 4, solid line is the Raman curve of graphene oxide, and dotted line is the Raman curve of hole Graphene, can be with from figure
See GO and RGO all characteristic peak D peak (~1350cm with Graphene-1) and G peaks (~1580cm-1)；The D peak intensities of RGO with
The ratio of G peak intensities is weak compared with GO, and defect is reduced after illustrating heat treatment reduction.
The test of specific surface area and pore analysis, as shown in Figure 6,6-a is using Brunauer-Emmett-Teller
(BET) method test, it is 536.155m this time to measure the specific surface area for obtaining2/g；6-b figures are corresponding pore analysis figures, are used
Barret-Joyner-Halenda (BJH) method is tested, and it is 1.28-44.6nm that data analysis provides hole distribution, from figure
In it can be seen that pore size be mainly distributed on 1.28-13.5nm.
Embodiment 2
Step a, graphene oxide being prepared with improving Hummers methods, and being separated into suspension with deionized water, concentration is
10mg/mL。
Step b, the graphene oxide suspension in step a is evenly coated on smooth sheet glass, being placed on temperature is
In 55 DEG C of thermostatic drying chamber, allow moisture evaporation to fall, dry film tears it down afterwards, that is, obtain that surface is smooth and interlayer is caused
Close graphene oxide paper.
Under step c, air atmosphere, warm table is preheated, temperature adjustment to 250 DEG C, after after temperature stabilization, by step b
In graphene oxide paper be directly placed on warm table.Wait about 2-3 seconds, you can the graphene oxide for being reduced, i.e.,
Nano aperture graphene paper.As shown in Figure 7,7-a is the smooth graphene oxide paper in filemot surface (GO), and 7-b is black
The shaggy nano aperture graphene paper (RGO) of color expansion.7-c, 7-d are respectively graphene oxide (GO) and nano aperture
Optical photograph of the cross section of graphene paper (RGO) under 50 times of enlargement ratios of light microscope.Illustrate that heat treatment process is produced
Obvious thermal expansion phenomenon.
It is the test of specific surface area and pore analysis in Fig. 8,8-a is using Brunauer-Emmett-Teller (BET)
Method is tested, and it is 286.048m this time to measure the specific surface area for obtaining2/g；8-b figures are corresponding pore analysis figures, are used
Barret-Joyner-Halenda (BJH) method is tested, and it is 1.75-43.1nm that data analysis provides hole distribution, from figure
In it can be seen that pore size be mainly distributed on 1.75-13.3nm.
Embodiment 3
Step a, graphene oxide being prepared with improving Hummers methods, and being separated into suspension with deionized water, concentration is
10mg/mL。
Step b, by the graphene oxide suspension freeze-drying in step a：Graphene oxide suspension is first placed on ice
Solid is frozen into case, is placed into during cold well temperature has reached -50 DEG C of freeze drier and is dried, you can obtain graphene oxide
Aeroge, the brown column aeroge solid as shown in Fig. 9-a.
Under step c, air atmosphere, warm table is preheated, temperature adjustment to 200 DEG C, after after temperature stabilization, by step b
In graphite oxide aerogel be directly placed on warm table.Wait about 3-5 seconds, graphite oxide aerogel adds from contact
The contact point of thermal station starts burning and with swelling, to the burning of whole aeroge totally, burn time duration about 0.01s.
Obtain the nano aperture graphene aerogel of the black as shown in Fig. 9-b.
It is the test of specific surface area and pore analysis in Figure 10,10-a is using Brunauer-Emmett-Teller
(BET) method test, it is 420.028m this time to measure the specific surface area for obtaining2/g；10-b figures are corresponding pore analysis figures, are used
Barret-Joyner-Halenda (BJH) method is tested, and it is 1.86-41.27nm that data analysis provides hole distribution, from
It can be seen that pore size is mainly distributed on 1.86-13.1nm in figure.
Claims (7)
1. a kind of method that thermo-contact formula prepares nano aperture Graphene, it is characterised in that carry out as follows：
Step a, by graphene oxide dispersion in deionized water, obtain graphene oxide suspension；
Step b, freeze-drying is carried out to graphene oxide suspension, obtain graphite oxide aerogel；
Or freeze-day with constant temperature is carried out to graphene oxide suspension, obtain graphene oxide paper；
Step c, in air atmosphere, by heat source be preheated to 200 DEG C and more than, after stabilizing the temperature, by the oxidation stone
Black alkene aeroge is placed on heat source, makes graphite oxide aerogel burning expansion, and graphene oxide is reduced, that is, received
Metre hole hole graphene aerogel；
Or in air atmosphere, by heat source be preheated to 200 DEG C and more than, after stabilizing the temperature, by the graphene oxide
Paper is placed on heat source, makes graphene oxide paper burning expansion, and graphene oxide is reduced, that is, obtain nano aperture Graphene
Paper.
2. the method that thermo-contact formula according to claim 1 prepares nano aperture Graphene, it is characterised in that：Step a institutes
The concentration for stating graphene oxide suspension is 4~10mg/mL.
3. the method that thermo-contact formula according to claim 1 prepares nano aperture Graphene, it is characterised in that：Step b institutes
Stating freeze-drying is carried out under conditions of -40 DEG C~-60 DEG C.
4. the method that thermo-contact formula according to claim 1 prepares nano aperture Graphene, it is characterised in that：Step b institutes
Stating freeze-day with constant temperature is carried out under conditions of 50 DEG C~65 DEG C.
5. the method that thermo-contact formula according to claim 1 prepares nano aperture Graphene, it is characterised in that：Step c institutes
Heat source is stated for warm table, tube furnace, electric hot plate or electromagnetic oven.
6. the method that thermo-contact formula according to claim 1 prepares nano aperture Graphene, it is characterised in that：Graphite oxide
Alkene aeroge or graphene oxide paper are placed on 0.01~3s on heat source, that is, complete burning expansion.
7. the method that thermo-contact formula according to claim 1 prepares nano aperture Graphene, it is characterised in that：Gained nanometer
Between 1.5nm-100nm, specific surface area exists the nano aperture scope of hole graphene aerogel or nano aperture graphene paper
280-1000m2Between/g.
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| CN105914056B (en) * | 2016-04-20 | 2018-04-20 | 青岛华高墨烯科技股份有限公司 | A kind of preparation method of graphene/nickel foam composite electrode |
| CN107311152B (en) * | 2016-04-27 | 2019-07-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Graphene aerogel, preparation method and application |
| CN106809821B (en) * | 2017-01-19 | 2018-09-11 | 广东烛光新能源科技有限公司 | The preparation method of graphene |
| CN108751181B (en) * | 2018-07-03 | 2020-01-14 | 清华大学 | Preparation method of heterostructure porous graphene oxide membrane, graphene membrane and generator |
| TWI718684B (en) * | 2019-09-26 | 2021-02-11 | 崑山科技大學 | Manufacturing for a graphite oxide aerogel and application thereof |
| CN112687476B (en) * | 2019-10-18 | 2022-06-10 | 昆山科技大学 | Preparation and application of graphene oxide carbon aerogel |
| CN111204740A (en) * | 2020-01-14 | 2020-05-29 | 大同煤矿集团有限责任公司 | Method for rapidly preparing graphene macroscopic body through self-propagating combustion |
| CN111422856A (en) * | 2020-04-03 | 2020-07-17 | 常州富烯科技股份有限公司 | Method for flame reduction of graphene oxide film and preparation method of graphene film |
| CN115676819A (en) * | 2021-07-21 | 2023-02-03 | 比亚迪股份有限公司 | Graphite material preparation method, graphite material and power battery |
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