CN107867680A - The preparation method and hydrogen peroxide Application in Sensing of individual layer self-supporting three-dimensional grapheme based on continuously shaped template method - Google Patents
The preparation method and hydrogen peroxide Application in Sensing of individual layer self-supporting three-dimensional grapheme based on continuously shaped template method Download PDFInfo
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- CN107867680A CN107867680A CN201711047099.0A CN201711047099A CN107867680A CN 107867680 A CN107867680 A CN 107867680A CN 201711047099 A CN201711047099 A CN 201711047099A CN 107867680 A CN107867680 A CN 107867680A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention discloses the preparation method and hydrogen peroxide Application in Sensing of the individual layer self-supporting three-dimensional grapheme based on continuously shaped template method, its main preparation process is, the mantoquita and organic matter mechanical mixture that decomposition temperature and fusing point are adapted to are uniform, it is then placed in mould and is pressed into blank, two temperature section calcination in mixed atmosphere is placed in again, obtain the three-dimensional manometer copper mold plate of macroscopical bulk and the individual layer three-dimensional grapheme in its superficial growth, then with corrosive liquids copper substrate corrosion is obtained into aperture mainly in 100 nanometers of self-supporting grapheme foam after cleaning.Due to great inner surface, a large amount of active materials can be loaded, therefore there is very high potential in terms of ultracapacitor and lithium electricity, also can modified biological active material be used for biological detection as electrode, and the present invention produces avtive spot because of the presence of graphene sheet layer edge and geometrical defect, in the case where not modifying, i.e., there is good response to hydrogen peroxide, it can be configured such that graphene copper compound sensor, the detection for hydrogen peroxide.
Description
Technical field
The invention belongs to the preparing technical field of nano material, is related to a kind of individual layer self-supporting three-dimensional grapheme nanometer foam
Preparation method and application.
Background technology
Graphene is the monolithic layer two-dimensional material that the carbon atom arrangement of sp2 hydridization is formed in honeycomb type lattice structure, only
There is the thickness of a carbon atom, be known most thin material, along with its unique big pi bond structure is made it have as highly conductive
Property, the number of advantages such as high-specific surface area, high-termal conductivity and excellent mechanical performance, absorption, catalysis, sensing, energy conversion with
The field such as storage and biological medicine all has good application prospect；Effect yet with powerful van der waals force makes
Irreversible aggregation easily occurs between graphene sheet layer that must be independent, reduces its specific surface area, and high piece interlayer contact
Resistance reduces its electric conductivity, so as to limit its application.
In order to make full use of the performance of graphene, it will be generally connected to each other between graphene film and be prepared into tridimensional network
So as to prevent its aggregation.Typically there are two methods, directly with carbon source for growth or graphene oxide, graphene sheet layer from group
Dress.After wherein self-assembly method mainly disperses graphene oxide, make graphene by processes such as gelation, reduction, dryings
Lamella connects to obtain three-dimensional grapheme by physically or chemically acting on.Another ripe method is with three-dimensional porous metal
It is that carbon source progress chemical vapor deposition obtains foamy graphite alkene with methane, ethanol etc. or metal oxide is substrate.Compare and
Speech, the graphene conductive of chemical crosslinking better than physical crosslinking graphene, the graphene of chemical vapor deposition growth then due to
Carbon atom is continuous and more preferable than the self assembly graphene conductive performance of chemistry or physical action connection.The three-dimensional stone prepared
Black another key of alkene foam is control pore structure, that is, controls the graphene number of plies and aperture.Common nickel substrate method growth, due to
The limitation of growth graphene principle causes the graphene number of plies to be difficult to control, and is readily obtained the more graphene of the number of plies, cannot be single
The three-dimensional grapheme of layer, limits its specific surface area.And copper is readily obtained the stone of individual layer or a small number of layers due to being self-limiting growth
Black alkene, but commercial foam copper aperture is all in hundreds of microns, even if having grown the number of plies controls good graphene, due to aperture too
Big and later stage corrosive liquid surface tension also is difficult to form self supporting structure, in order to solve this problem, we select continuously into
Type lumpy nanometer copper mold plate simultaneously goes out that the number of plies is few, specific surface area is big as substrate growth, the small three-dimensional stone for being capable of self-supporting in aperture
Black alkene nanometer foam.
Mantoquita decomposition or copper oxide nanometer particle, which are sintered, can obtain the foam copper of nano aperture, but the fusing point of copper
The growth temperature of graphene is only slightly higher than, and because its nanostructured also has great surface area and surface energy, causes it
It is unstable at high temperature, there is greatly polymerization tendency between nano particle, cause it to form copper billet, nano-void less at high temperature
Disappear, so as to not have the effect as nanometer foam substrate, so traditional gaseous carbon source or liquid carbon source can not all give birth to
Grow required graphene.Based on problem above, the mantoquita and solid organic of adaptation are well mixed by the present invention, in advance pressure
Required shape is made, while most micron order macropore, the then calcination under mixed atmosphere, liquid are eliminated by suppressing
Small organic molecule or the macromolecule organic of viscous state flowed when mantoquita decomposes and is reduced to Nanometer Copper foam
Its surface is covered in, prevents it to polymerize while plays cementation, help forms Nanometer Copper foam, while advance compacting
So that its controlled shape rather than scattered powdered, obtains the nanometer foam copper of bulk, then rises to high temperature, in situ point of organic matter
Solution obtains three-dimensional grapheme nanometer foam.Selection according further to carbon source can prepare intrinsic graphene or doped graphene,
And due to its self supporting structure, itself can serve as electrode material, so as to simplify the preparation of electrode, resulting electrode by
Few and huger than surface in the graphene number of plies, aperture is small to be beneficial to self-supporting and provides more active attachment sites, is advantageous to
Its application in terms of lithium electricity, ultracapacitor and catalysis.
The content of the invention
The present invention is intended to provide a kind of raw material sources are cheap extensively, and operating method simple and fast, with short production cycle and efficiency
The preparation method and applications of high individual layer self-supporting three-dimensional grapheme nanometer foam；The individual layer three-dimensional stone that the present invention prepares
Black alkene nanometer foam, primary aperture can be controlled by this method at nanoscale (less than 100 nanometers), overcome Commercial foam copper
The shortcomings that being caved in for the individual layer blocky graphite alkene of substrate grown in etching process, reach the purpose of self-supporting.
The preparation method of the individual layer self-supporting three-dimensional grapheme nanometer foam of the present invention, is to use continuously shaped template method,
Preparation process includes：The mantoquita of adaptation and organic matter carbon source mechanical mixture is uniform, it is then placed in mould and is suppressed with hydraulic press
Blank is obtained, then is placed in two temperature section calcination in mixed atmosphere, obtains the individual layer three-dimensional graphite in its superficial growth of macroscopical bulk
The three-dimensional manometer copper mold plate of alkene, then with corrosive liquids copper substrate corrosion is obtained into individual layer self-supporting three-dimensional graphite after cleaning
Alkene nanometer foam.
In above-mentioned technical proposal, described mantoquita decomposes mantoquita using easy, included but is not limited to as copper source decomposition-reduction
Basic copper carbonate, copper acetate, copper sulphate, copper nitrate or cupric oxalate.
Described organic matter carbon source and mantoquita adaptation, selected carbon source is linear polymeric organic matter or small organic molecule,
Its fusing point is below mantoquita decomposition temperature if small organic molecule is selected, and boiling point is more than mantoquita decomposition temperature, if selection line
Property macromolecule organic, then its flow temperature below corresponding mantoquita decomposition temperature and its decomposition temperature mantoquita decomposition temperature it
On.
Described small organic molecule is the polar organic matter containing hydrogen bond or can be including but unlimited into the organic matter of inner salt
In phthalic anhydride, phenylenediamine or p-aminobenzoic acid.
Described linear polymeric organic matter is linear polymer, including but not limited to PMMA or polyamide series.
Described organic matter carbon source and mantoquita in mass ratio 1~10:20 carry out grinding mixing, different according to carbon source property,
Mantoquita can also be ground in advance and be mixed again with carbon source, milling time is preferably 5 to 60 minutes.
Described hydraulic press is using manually or automatically, and pressure is 10 to 40 MPas during compacting, and the press time is 5 to arrive 60min,
According to blank be molded and be stripped situation can with spray-on process additive polarity solvent improve shaping situation, solvent for use include ethanol, acetone,
Or ethylene glycol etc..Compacting can preforming graphene shape, while reduce internal micron order cavity, auxiliary control aperture.It is selected
Mould can be stainless steel or Carbon Steel Die, in mold cavity shape can be it is circular either square or any required for shape
Shape, last prepared three-dimensional grapheme shape depend on the volume and shape of institute's slug press.
Two described temperature section calcinations refer to：By blank as under mixed atmosphere, using heating rate as 5-20 DEG C of liter per minute
Temperature is incubated 30-240 minutes, mantoquita is gradually decomposed into copper oxide nanometer particle and escaping gas, simultaneously to mantoquita decomposition temperature
It is reduced to copper nano particles and is connected to each other to the lumpy nanometer copper mold plate with pre-stamped profile, and now small molecule is organic
Thing is in liquid, or linear polymeric is in viscous state, will attach to the inner surface of Nanometer Copper foam, both replicates foam copper
Pattern also function to buffer action, will prevent copper from sintering solid copper billet into follow-up pyroprocess；Continue every with 10-50 DEG C
Minute is warming up to 700-1050 DEG C, is incubated 30-180 minutes, is subsequently cooled to room temperature, and in section heating, be attached to surface has
Machine thing is gradually decomposed into carbon atom on copper surface, and the generation graphene that is connected to each other in temperature-fall period；Described mixed gas
For the mixing of hydrogen and any inert gas, inert gas includes argon gas, nitrogen, helium, and wherein hydrogen flowing quantity is 25-
500sccm, inert gas flow 50-1000sccm.After blank calcination, can continuously shaped aperture below 100 nanometers
Foam copper substrate and the foamy graphite alkene as template.
Described corrosive liquids includes hydrogen peroxide hydrochloric acid mixed solution, potassium permanganate sulfuric acid mixture liquid or iron chloride hydrochloric acid
Mixed liquor etc..
Individual layer self-supporting three-dimensional grapheme nanometer foam made from the above method has the spies such as the big, high conductivity of specific surface area
Point, there is graded porous structure, a small number of macropores are in micron level, and primary aperture is below 100 nanometers, compared to traditional nickel foam
The three-dimensional grapheme of substrate CVD growth, can more effectively control the graphene number of plies, greatly reduce aperture, reduce hole
Volume, is effectively utilized the inner space of self-supporting graphene, and key is to realize individual layer three by the technique of simple economy
Tie up the self-supporting of graphene.The three-dimensional grapheme nanometer foam of the present invention is due to that with great inner surface, can load a large amount of work
Property material, therefore have very high potential in terms of ultracapacitor and lithium electricity, also can modified biological active material be used for as electrode
Biological detection, in addition, the graphene nano foam of the present invention produces because of the presence of graphene sheet layer edge and geometrical defect
Avtive spot, reservation copper is collector, in the case where not modifying, i.e., has good response to hydrogen peroxide, sensitivity can be high
Up to for 500 μ A/M/cm2, can be configured such that graphene copper compound sensor, the detection for hydrogen peroxide.
Brief description of the drawings
Three-dimensional grapheme SEM figures prepared by Fig. 1 embodiments 1；
Three-dimensional grapheme SEM figures prepared by Fig. 2 embodiments 2；
Three-dimensional grapheme SEM figures prepared by Fig. 3 embodiments 3；
Fig. 4 embodiments 3 are used for the IT curves of hydrogen peroxide detection.
Embodiment
With reference to specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.
Embodiment 1
1. taking basic copper carbonate 0.2g, PMMA0.05g, 15min is fully ground, a small amount of absolute ethyl alcohol is sprayed and is well mixed,
It is placed in the interior diameter 1.4cm cylindrical die of cleaning, hydraulic press center is placed in after matched moulds, boosts to 20MPa, and keep
Taken out after 25min.
It is placed in 2. blank quartz boat is loaded in quartz ampoule, after discharging air, adjusts hydrogen flowing quantity 50sccm, argon gas stream
100sccm is measured, 250 DEG C are warming up to 5 DEG C/min speed, is incubated 2h, then 900 DEG C are warming up to 15 DEG C/min speed, is protected
Room temperature is down to after warm 1h.
3. burnt sample is placed in hydrogen peroxide and hydrochloric acid 1:In the mixed solution of 2 (volume ratios), corrode at 70 DEG C
In one evening, fully cleaned with deionized water within second day and obtain three-dimensional grapheme.
4. taking the sample after calcination to be cut directly into 1cm × 0.5cm small pieces, the electrochemistry that can be directly used for hydrogen peroxide is visited
Survey.
Embodiment 2
1. taking basic copper carbonate 0.2g, p-aminobenzoic acid 0.06g, 15min is fully ground, sprays a small amount of absolute ethyl alcohol and mix
Close uniformly, be placed in the interior diameter 1.4cm cylindrical die of cleaning, hydraulic press center is placed in after matched moulds, boosts to 15MPa,
And taken out after keeping 30min.
It is placed in 2. blank quartz boat is loaded in quartz ampoule, after discharging air, adjusts hydrogen flowing quantity 100sccm, argon gas
Flow 100sccm, 280 DEG C are warming up to 10 DEG C/min speed, is incubated 1.5h, then 1000 are warming up to 15 DEG C/min speed
DEG C, it is down to room temperature after being incubated 1.5h.
3. burnt sample is taken to be placed in hydrogen peroxide and hydrochloric acid 1:In the mixed solution of 2 (volume ratios), corrode at 70 DEG C
In one evening, fully cleaned with deionized water within second day and obtain three-dimensional grapheme.
4. taking the sample after calcination to be cut directly into 1cm × 0.5cm small pieces, the electrochemistry that can be directly used for hydrogen peroxide is visited
Survey.
Embodiment 3
1. taking copper acetate 0.2g, to PA120.04g, 20min is fully ground, and is well mixed, is placed in the interior diameter of cleaning
Hydraulic press center is placed in 1.4cm cylindrical die, after matched moulds, boosts to 20MPa, and is taken out after keeping 10min.
It is placed in 2. blank quartz boat is loaded in quartz ampoule, after discharging air, adjusts hydrogen flowing quantity 150sccm, argon gas
Flow 200sccm, 300 DEG C are warming up to 10 DEG C/min speed, is incubated 2.5h, then 950 are warming up to 15 DEG C/min speed
DEG C, it is down to room temperature after being incubated 2h.
3. burnt sample is taken to be placed in hydrogen peroxide and hydrochloric acid 1:In the mixed solution of 2 (volume ratios), corrode at 70 DEG C
In one evening, fully cleaned with deionized water within second day and obtain three-dimensional grapheme.
4. taking the sample after calcination to be cut directly into 1cm × 0.5cm small pieces, the electrochemistry that can be directly used for hydrogen peroxide is visited
Survey.
Claims (10)
1. a kind of preparation method of individual layer self-supporting three-dimensional grapheme nanometer foam, it is characterised in that use continuously shaped template
Method, preparation process include：The mantoquita of adaptation and organic matter carbon source mechanical mixture is uniform, it is then placed in mould with hydraulic press pressure
Blank is made, then is placed in two temperature section calcination in mixed atmosphere, obtains the individual layer three-dimensional stone in its superficial growth of macroscopical bulk
The three-dimensional manometer copper mold plate of black alkene, then with corrosive liquids copper substrate corrosion is obtained into individual layer self-supporting three-dimensional stone after cleaning
Black alkene nanometer foam.
2. the preparation method of individual layer self-supporting three-dimensional grapheme nanometer foam according to claim 1, it is characterised in that institute
The mantoquita stated decomposes mantoquita as copper source decomposition-reduction, using easy, including basic copper carbonate, copper acetate, copper sulphate, copper nitrate,
Or cupric oxalate.
3. the preparation method of individual layer self-supporting three-dimensional grapheme nanometer foam according to claim 1, it is characterised in that institute
Organic matter carbon source and the mantoquita adaptation stated, selected carbon source is linear polymeric organic matter or small organic molecule, if small point of selection
Then its fusing point is below mantoquita decomposition temperature for sub- organic matter, and boiling point is more than mantoquita decomposition temperature, if selection linear polymeric has
Machine thing, then its flow temperature below corresponding mantoquita decomposition temperature and its decomposition temperature on mantoquita decomposition temperature.
4. the preparation method of individual layer self-supporting three-dimensional grapheme nanometer foam according to claim 3, it is characterised in that institute
The small organic molecule stated is the polar organic matter containing hydrogen bond or can be into the organic matter of inner salt, including phthalic anhydride, benzene
Diamines or p-aminobenzoic acid.
5. the preparation method of individual layer self-supporting three-dimensional grapheme nanometer foam according to claim 3, it is characterised in that institute
The linear polymeric organic matter stated is linear polymer, including PMMA or polyamide series.
6. the preparation method of individual layer self-supporting three-dimensional grapheme nanometer foam according to claim 1, it is characterised in that institute
The organic matter carbon source and mantoquita in mass ratio 1~10 stated:20 carry out grinding mixing.
7. the preparation method of individual layer self-supporting three-dimensional grapheme nanometer foam according to claim 1, it is characterised in that institute
Pressure is 10 to 40 MPas during the hydraulic press compacting stated, and the press time arrives 60min for 5, and being molded according to blank and be stripped situation can
Shaping situation is improved with spray-on process additive polarity solvent, solvent for use includes ethanol, acetone or ethylene glycol.
8. the preparation method of the individual layer self-supporting three-dimensional grapheme nanometer foam described in claim 1, it is characterised in that described
Two temperature section calcinations refer to：By blank as under mixed atmosphere, temperature is decomposed by the 5-20 DEG C of mantoquita per minute that is warming up to of heating rate
Degree, be incubated 30-240 minutes, continue with 10-50 DEG C it is per minute be warming up to 700-1050 DEG C, be incubated 30-180 minutes, then cool down
To room temperature；Described mixed gas is the mixing of hydrogen and any inert gas, and inert gas includes argon gas, nitrogen, helium, its
Middle hydrogen flowing quantity is 25-500sccm, inert gas flow 50-1000sccm.
9. the preparation method of individual layer self-supporting three-dimensional grapheme nanometer foam according to claim 1, it is characterised in that institute
The corrosive liquids stated includes hydrogen peroxide hydrochloric acid mixed solution, potassium permanganate sulfuric acid mixture liquid or iron chloride hydrochloric acid mixed solution.
10. the individual layer self-supporting three-dimensional grapheme nanometer foam that the method as described in claim any one of 1-9 prepares
Using, it is characterised in that described individual layer self-supporting three-dimensional grapheme nanometer foam is used for the spy of hydrogen peroxide directly as electrode
Survey, sensitivity is 500 μ A/M/cm2。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109365799A (en) * | 2018-09-19 | 2019-02-22 | 上海新池能源科技有限公司 | Preparation method and Metal Substrate-graphene electric contact of graphene coated metal-powder |
| CN109365799B (en) * | 2018-09-19 | 2024-04-23 | 上海新池能源科技有限公司 | Preparation method of graphene coated metal powder and metal-based-graphene electrical contact |
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| CN106521204A (en) * | 2016-12-16 | 2017-03-22 | 天津大学 | Preparation method of in-situ grown graphene reinforced metal-based composite material |
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| CN109365799A (en) * | 2018-09-19 | 2019-02-22 | 上海新池能源科技有限公司 | Preparation method and Metal Substrate-graphene electric contact of graphene coated metal-powder |
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