CN106006615A - Natural drying preparation method of graphene aerogel - Google Patents
Natural drying preparation method of graphene aerogel Download PDFInfo
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- CN106006615A CN106006615A CN201610352474.1A CN201610352474A CN106006615A CN 106006615 A CN106006615 A CN 106006615A CN 201610352474 A CN201610352474 A CN 201610352474A CN 106006615 A CN106006615 A CN 106006615A
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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
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Abstract
The invention provides a natural drying preparation method of graphene aerogel. The method comprises the following steps: mixing a graphene oxide solution with a reducing agent ethylenediamine (EDA) and borax, wherein hydrogel is formed by self-assembly after a period of time of hydrothermal reaction; performing dialysis and pre-freezing for a period of time for moulding; and drying to remove moisture to obtain the graphene aerogel with sound shape and without volume shrinkage. In the invention, through the improved hydrothermal reaction and a bionic means (borate crosslinking effect) between the graphene sheet layers, the rigidity of the aerogel is enhanced, the contact angle between water and graphene is controlled, and the capillary force in the drying process is remarkably reduced. In the invention, the preparation process is simple and easy to control, the production cost is low, and batch production is easy to implement; the prepared graphene aerogel has excellent mechanical property and the like; and a technical support is provided for large-scale commercial preparation of graphene aerogel.
Description
Technical field
The present invention relates to the energy and field of new, be specifically related to a kind of graphene aerogel natural drying preparation method.
Background technology
Graphene aerogel (Graphene Aerogel) due to the electric conductivity (～10S/cm) of its excellence, interesting super-elasticity (～99%), bigger serface (～840m2/ g), the porosity (～99%) such as superelevation, extremely low density (～10mg/cm3), a series of performances such as oleophylic fire prevention, there is huge potential application in fields such as the energy, environmental protection, catalyst carriers.By using graphene oxide (GO) as presoma, by the gradually reduction to GO lamella, make progressively disengaging of the substantial amounts of oxy radical in its surface, reduce the electrostatic repulsion of sheet interlayer and promote it and mutually overlap and form stable three-dimensional overall hydrogel structure, then hydrogel internal solvent is removed by lyophilization or supercritical drying i.e. can get Graphene three-dimensional aerogel structure.The most conventional graphene aerogel preparation method mainly has: assemble in situ method, induces construction from part, chemical crosslink technique.
Assemble in situ method is by the gradually reduction to graphene oxide lamella so that the substantial amounts of oxygen-containing functional group in its surface gradually removes, and reduces the electrostatic repulsion between lamella and promotes it and mutually overlap and form stable three-dimensional overall structure.Sun Litao et al. utilizes ammonia and the pH value of hydrochloric acid regulation and control graphene oxide dispersion, finds when the pH value of system is about 10, and the end product graphene aerogel obtained has the highest electrical conductivity and the highest mechanical strength.Qu Liangti et al. introduces pyrroles as swelling agent in the dispersion liquid of graphene oxide, reduces redox graphene nanometer sheet accumulation degree in an assembling process, graphene aerogel porosity is greatly improved.Cheng Huiming et al. has then obtained mechanical strength height, pore structure and surface chemical property adjustable graphene aerogel as additive by the assemble in situ that hydro-thermal assists using thiourea, this structure is to Some Organic Pollutants, and such as dyestuff, oil product and organic solvent etc. all show extraordinary characterization of adsorption.In addition to utilizing hydro-thermal and completing assemble in situ, use electronation approach also can realize this process.For hydro-thermal approach, electronation is gentle due to reaction condition, it is easier to realize extension preparation.Yan Lifeng et al. has investigated the probability of a series of reducing agent induction preparation Graphene gel, and result of study shows NaHSO3、Na2The multiple reducing agent inorganic, organic such as S, HI and hydroquinone is respectively provided with redox graphene and prepares the potentiality of graphene aerogel.Zhang Xuetong et al. proposes to utilize ascorbic acid for reducing agent, and under conditions of without external disturbance, redox graphene is after reaction was more than 2 hours, just can form the gel structure with good mechanical strength.
Induction construction from part is by under extraneous inducing action, and the balance of graphene oxide colloidal dispersion system is broken, and forms Graphene gel structure when it reaches new balance.Seo et al. utilizes traditional vacuum technological guide graphene oxide to assemble.In this process, the effect of centrifugal force can promote graphene oxide to be enriched with, and under vacuum condition, evaporation of water then can make graphene oxide form loose structure in banking process.By heat treatment subsequently, i.e. can get graphene aerogel.Kim et al. employing breath pattern method induced oxidation Graphene carries out assembling and prepares the graphene aerogel of ordered big hole structure.In addition to water droplet, ice crystal also can the assembling of effective induced oxidation Graphene.Li et al. takes the lead in using ascorbic acid that graphene oxide carries out the reduction of part, in refrigerating process subsequently, the formation of ice can cause the dissolubility of these graphene films to reduce, and separates out from liquid phase, and assemble round the surrounding of ice crystal, obtain that there is anisotropic ordered structure；The graphene aerogel having obtained there is ordered big hole is being processed through follow-up dry and drastic reduction.
Chemical crosslink technique is to introduce chemical crosslinking between lamella by other component of addition further during preparing gel at graphene oxide to come modulation graphene aerogel structure and character.Graphene oxide and glucose are carried out common hydro-thermal by Wang Xun et al., and glucose can form chemical crosslinking due to polycondensation between graphene sheet layer, has obtained the graphene aerogel structure of high mechanical properties.Worsley et al. introduces phenol and formaldehyde in the aqueous solution of graphene oxide and utilizes sodium carbonate as the polymerization of catalyst inducement phenol and formaldehyde by crosslinked together for stannic oxide/graphene nano sheet；Carbonization treatment subsequently makes phenolic resin be converted into carbon and form crosslinking between graphene sheet layer.
In sum, graphene three-dimensional structure construction method generally exists limited by the dry preparation condition in harshness and cause at present cannot large scale, large-scale production and application.The graphene three-dimensional structure that graphene aerogel produces as wherein applicable large scale with GO as presoma, owing to hydrogel backbone internal solvent exists surface tension, can produce under natural drying skeleton subside and the contraction of volume and form xerogel, the most all need to use Freeze Drying Technique or Supercritical Drying Technology to the moisture removing in graphene-structured.But, either cryogenic vacuum condition or the condition of high voltage needed for supercritical drying needed for lyophilization increase the production cost of graphene aerogel of knowing clearly, difficulty the most largely, and limit its macro-size.
Summary of the invention
Based on above weak point, it is an object of the invention to provide a kind of graphene aerogel natural drying preparation method, can possess that production cost is low, preparation difficulty advantage low, that set without special producing.
The technology used in the present invention method is as follows: a kind of graphene aerogel natural drying preparation method, it is as follows: after graphene oxide solution is mixed with reducing agent ethylenediamine EDA and Borax, it is self-assembly of hydrogel by hydro-thermal reaction a period of time, again through dialysis, the molding of pre-freeze a period of time further, finally it is dried and the removing of wherein moisture is obtained the intact graphene aerogel without volume contraction of shape.
The present invention also has a following technical characteristic:
1, graphene oxide solution concentration as above is 5mg/ml.
2, it is 5% Borax Na by graphene oxide solution that 10ml concentration is 5mg/ml with 60 μm reducing agent ethylenediamine EDA and 50 μm mass fractions2B4O7Solution mixes.
3, hydro-thermal reaction as above is 120 DEG C of hydro-thermal reactions 14 hours.
4, dialysis as above uses volume fraction to be 1% ethanol water.
5, pre-freeze 12 hours in-10 DEG C it are placed in as above.
6, a kind of graphene aerogel natural drying preparation method as above, step is as follows:
Step one: be 5% Borax Na with 60 μm reducing agent ethylenediamine EDA and 50 μm mass fractions by graphene oxide solution that 10ml concentration is 5mg/ml2B4O7Solution mixes, and by mixed liquor ultrasonic disperse 30 minutes, takes 1ml mixed liquor in 5ml container bottle, container bottle is put into 120 DEG C of reactions in reactor and within 14 hours, forms hydrogel；
Step 2: be that 1% ethanol water was dialysed after 6 hours by hydrogel volume fraction obtained above, it is placed in pre-freeze 12 hours in-10 DEG C of refrigerators, finally the hydrogel taking-up after freezing is dried 24 hours at normal temperatures and pressures and obtains the intact graphene aerogel without volume contraction of shape.
The natural drying preparation method of the graphene aerogel that the present invention relates to, possess that preparation cost is low, difficulty is little, without the advantage such as special installation and energy-conserving and environment-protective, alternative lyophilization and Supercritical Drying Technology, promote extensive, the large scale preparation of graphene aerogel and at flexible robot, driver, sensor, electrode and ultracapacitor, ultralight protective material, the application in the field such as insulation and environmental improvement.
Accompanying drawing explanation
Fig. 1 be natural drying prepare graphene aerogel structure SEM, TEM photo；Graphite aeroge SEM figure prepared by (a) natural drying；B () graphene aerogel core space SEM schemes；C () graphene aerogel marginal zone SEM schemes；D () graphene aerogel transition region SEM is schemed；E () graphene aerogel rupture zone SEM schemes；F () pore wall thickness SEM schemes；(g) hole wall TEM figure (h-i) hole wall join domain high magnification TEM figure；
Fig. 2 is graphene aerogel mechanical property investigation and comparison figure prepared by natural drying；A () longitudinal pressurized can recovery strain 99% figure, front 5 compression chords-strain curve figure of (b) natural drying graphene aerogel compression 50%, c natural drying aeroge prepared by () different GO concentration is the stress-strain curve of 99% in decrement, the limit stress in the circulation of (d) 100 second compression, single energy loss, Young's modulus change curve；
Fig. 3 is the graphene aerogel electricity prepared of natural drying and thermal property investigation and comparison figure；(a) graphene aerogel conductivity test figure, (b) piezoresistive effect test figure, (c) Determination of conductive coefficients figure, (d) heat stability testing figure.
Detailed description of the invention
Illustrate below in conjunction with the accompanying drawings and patent of the present invention be described in more detail:
Embodiment 1:
The preparation method of a kind of graphene aerogel natural drying is as follows:
1) it is 5% Borax (Na by graphene oxide solution that 10ml concentration is 5mg/ml with 60 μm reducing agent ethylenediamine (EDA) and 50 μm mass fractions2B4O7) solution mixing, by mixed liquor ultrasonic disperse 30 minutes, take 1ml mixed liquor in 5 ml container bottle, container bottle is put into 120 DEG C of hydro-thermal reactions in reactor and within 14 hours, forms hydrogel.
2) it is that 1% ethanol water was dialysed after 6 hours by hydrogel volume fraction obtained above, it is placed in-10 DEG C of refrigerators freezing 12 hours, finally the hydrogel taking-up (normal temperature and pressure) under field conditions (factors) after freezing is dried and within 24 hours, obtains the intact graphene aerogel shunk without large volume of shape.Graphene aerogel volume contraction in natural drying process and skeleton all can be subsided to cause and be significantly affected by graphene oxide solution concentration, hydrothermal reduction time, dialysis solution water alcohol ratio and pre-freezing temperature.The parameter that the present invention relates to, controls when more than 4mg/ml, 14 hours hydrothermal reduction time, dialysis solution water alcohol volume ratio 1%, it is possible to successfully prepare the shrinkage-free graphene aerogel of volume by graphene oxide concentration.Reduce hydrothermal reduction time and pre-freezing temperature, or increase dialysis solution water alcohol ratio, graphene aerogel all can be caused to produce volume contraction in various degree or structure collapses.
Embodiment 2:
In conjunction with Fig. 1, natural drying method prepares inner porosity SEM, TEM characterization test of graphene aerogel, as follows:
The graphene aerogel natural drying preparation method that the present invention proposes reduction based on produced capillary force that solvent is volatilized naturally and the bionical enhancing of the rigidity of structure to aeroge own.Due to during pre-freeze ice-crystal growth to the effect of liquid capillary tension in the extruding of aerogel structure and natural drying process so that last graphene aerogel presents the shell-core structure of uniqueness, as shown in Figure 1a.This shell-core structure is made up of the middle part cellular nuclear structure of rule and peripheral loose shell structure.Wherein nuclear structure average cell size is 100 microns, and shell structure is 200 microns, as shown in Fig. 1 b-d.Fig. 1 e shows that the oversized hole structure of outer casing part is caused by the hole wall caused due to ice-crystal growth and solvent capillary force destroys.Fig. 1 f-i shows, natural drying method is prepared gained graphene aerogel structure and had thicker hole wall, is formed by about 70 layer graphene self assembly π-π overlap joints.
Embodiment 3:
In conjunction with Fig. 2, natural drying method prepares the Mechanics Performance Testing of graphene aerogel, as follows:
The graphene aerogel that the present invention uses natural drying method to prepare has the recovered compression deflection characteristics of up to 99%, and the limit stress of up to 1MPa, and as shown in Figure 2 a, this performance is the top level of current graphene aerogel research.Fig. 2 b shows that this graphene aerogel material possesses higher initiating structure rigidity, it is to avoid structure volume contraction in natural drying process because caused by capillary stress and structure collapses.By 100 CYCLIC LOADING to this material, it was demonstrated that this graphene aerogel possesses stable, excellent super-elasticity mechanical property, as shown in Fig. 2 c, d.
Embodiment 4:
In conjunction with Fig. 3, natural drying method prepares the electricity of graphene aerogel, thermal property test, as follows:
Graphene aerogel prepared by natural drying method possesses the electrical conductivity of up to 1.3S/cm, stable piezoresistive effect, and ultralow heat conductivity 0.018W/mK and the heat stability of excellence, as shown in Fig. 3 a-d.Above-mentioned electricity, thermal property are in the top level of current graphene aerogel performance study, show that the graphene aerogel natural drying method not only preparation cost that the present invention proposes is low, difficulty is little, and ensure that every excellent properties of aeroge, extensive, large scale preparation for graphene aerogel provide technical support.
Claims (7)
1. a graphene aerogel natural drying preparation method, it is characterised in that: by graphene oxide solution
After mixing with reducing agent ethylenediamine EDA and Borax, it is self-assembly of hydrogel by hydro-thermal reaction a period of time,
Again through dialysis, the molding of pre-freeze a period of time further, finally dry removing by wherein moisture obtains the intact nothing of shape
The graphene aerogel of volume contraction.
A kind of graphene aerogel natural drying preparation method the most according to claim 1, its feature exists
In, graphene oxide solution concentration is 5mg/ml.
A kind of graphene aerogel natural drying preparation method the most according to claim 1, its feature exists
In, by graphene oxide solution that 10ml concentration is 5mg/ml and 60 μm reducing agent ethylenediamine EDA and
50 μm mass fractions are 5% Borax Na2B4O7Solution mixes.
A kind of graphene aerogel natural drying preparation method the most according to claim 1, its feature exists
In, hydro-thermal reaction is 120 DEG C of hydro-thermal reactions 14 hours.
A kind of graphene aerogel natural drying preparation method the most according to claim 1, its feature exists
In, dialysis uses volume fraction to be 1% ethanol water.
A kind of graphene aerogel natural drying preparation method the most according to claim 1, its feature exists
In, it is placed in pre-freeze 12 hours in-10 DEG C.
A kind of graphene aerogel natural drying preparation method the most according to claim 1, its feature exists
In, step is as follows:
Step one: by graphene oxide solution and 60 μm reducing agent second two that 10ml concentration is 5mg/ml
Amine EDA and 50 μm mass fractions are 5% Borax Na2B4O7Solution mixes, by mixed liquor ultrasonic disperse 30
Minute, take 1ml mixed liquor in 5ml container bottle, container bottle is put into 120 DEG C of reactions 14 in reactor little
Time formed hydrogel；
Step 2: be that 1% ethanol water was dialysed after 6 hours by hydrogel volume fraction obtained above,
It is placed in pre-freeze 12 hours in-10 DEG C, finally the hydrogel taking-up after freezing is dried 24 at normal temperatures and pressures little
Time obtain the intact graphene aerogel without volume contraction of shape.
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Cited By (15)
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| CN106768508A (en) * | 2016-12-02 | 2017-05-31 | 西安交通大学 | A kind of gel capacitance type sensor and method for measuring plantar pressure and dynamic change |
| CN107226466A (en) * | 2017-08-01 | 2017-10-03 | 西南科技大学 | The method that nitrogen-doped graphene aeroge is prepared using plant extraction liquid modification |
| CN107311163A (en) * | 2017-07-05 | 2017-11-03 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of graphene composite porous charcoal |
| CN108423654A (en) * | 2018-03-28 | 2018-08-21 | 陕西科技大学 | A kind of amination graphene aeroge high-efficiency adsorbent, preparation method and applications |
| CN108615621A (en) * | 2018-06-22 | 2018-10-02 | 安徽大学 | A kind of composite graphite alkene silica aerogel electrode, preparation method and application |
| CN109437178A (en) * | 2018-12-06 | 2019-03-08 | 佛山科学技术学院 | A kind of green low-energy consumption preparation method of high strength graphite alkene aeroge |
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| CN106768508A (en) * | 2016-12-02 | 2017-05-31 | 西安交通大学 | A kind of gel capacitance type sensor and method for measuring plantar pressure and dynamic change |
| CN106768508B (en) * | 2016-12-02 | 2020-05-15 | 西安交通大学 | Gel capacitance type sensor and method for measuring plantar pressure and dynamic change |
| CN107311163A (en) * | 2017-07-05 | 2017-11-03 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of graphene composite porous charcoal |
| CN107311163B (en) * | 2017-07-05 | 2019-09-24 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of graphene composite porous charcoal |
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| CN107226466A (en) * | 2017-08-01 | 2017-10-03 | 西南科技大学 | The method that nitrogen-doped graphene aeroge is prepared using plant extraction liquid modification |
| CN108423654A (en) * | 2018-03-28 | 2018-08-21 | 陕西科技大学 | A kind of amination graphene aeroge high-efficiency adsorbent, preparation method and applications |
| CN108615621A (en) * | 2018-06-22 | 2018-10-02 | 安徽大学 | A kind of composite graphite alkene silica aerogel electrode, preparation method and application |
| CN109437178A (en) * | 2018-12-06 | 2019-03-08 | 佛山科学技术学院 | A kind of green low-energy consumption preparation method of high strength graphite alkene aeroge |
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| CN110155993B (en) * | 2019-06-27 | 2021-01-26 | 中素新科技有限公司 | Hydrophobic graphene aerogel and preparation method and application thereof |
| CN110155993A (en) * | 2019-06-27 | 2019-08-23 | 中素新科技有限公司 | Hydrophobic graphene aerogel and its preparation method and application |
| CN111252754B (en) * | 2020-03-12 | 2020-12-29 | 浙江大学 | Graphene aerogel air hole regulation and control method and graphene gradient aerogel |
| WO2021179232A1 (en) * | 2020-03-12 | 2021-09-16 | 浙江大学 | Method for preparing aerogel via solvent plasticization and foaming |
| CN111252754A (en) * | 2020-03-12 | 2020-06-09 | 浙江大学 | Graphene aerogel air hole regulation and control method and graphene gradient aerogel |
| CN112429721A (en) * | 2020-11-24 | 2021-03-02 | 安徽大学 | Composite graphene aerogel, preparation method and application of composite graphene aerogel in super-capacitor pressure sensor |
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| CN112794705A (en) * | 2021-01-13 | 2021-05-14 | 兰州大学 | Method for preparing hyperelastic silicon oxide nano ceramic aerogel based on graphene serving as template |
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