CN108178149A - A kind of preparation method of graphene nano volume - Google Patents
A kind of preparation method of graphene nano volume Download PDFInfo
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- CN108178149A CN108178149A CN201810120053.5A CN201810120053A CN108178149A CN 108178149 A CN108178149 A CN 108178149A CN 201810120053 A CN201810120053 A CN 201810120053A CN 108178149 A CN108178149 A CN 108178149A
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Abstract
The present invention relates to a kind of preparation methods of graphene nano volume, using redox graphene as raw material, under the cooperation of nano-particle, are rolled up by fricting shearing effect to obtain graphene nano.The present invention has larger selectivity to the material and shape of nano-particle, and the obtained separation of nanometer roll and nano-particle is also relatively easy to, and the preparation process of this method is simple, and the period is short and at low cost.
Description
Technical field
The present invention relates to technical field of film preparation, and in particular to a kind of preparation method of graphene nano volume.
Background technology
Carbon is a kind of most general element, there are a variety of allotropes, such as graphite, diamond and nanostructured
Fullerene, nanotube and graphene.Graphene causes extensive concern because of its unique performance.Graphene be by monolayer carbon with
Six-membered cyclic close-packed arrays and the lattice structure material of bi-dimensional cellular shape formed, many studies have shown that, it is special that graphene has
Photoelectric properties and physical and chemical performance.There is transparency height, good conductivity and specific surface area by film prepared by graphene
It is big to wait excellent properties.In addition, graphene can be as a kind of two-dimentional basic material of other dimension carbon nanomaterials, it can be by
The bucky-ball of zero dimension is rolled into, be curled into one-dimensional nanotube or is piled into three-dimensional graphite.People have prepared big face at present
Long-pending Sheet Graphite alkene, and stone can be obtained when the size reduction of graphene is to 20nm or so by further chemical shearing method
Black alkene quantum dot (GQDs), and rolled up when graphene can obtain graphene nano under certain driving effect by curling.However, mesh
The preceding research to graphene nano volume is less, and understanding is inadequate, and theoretical research report is also less, and Structure Mechanism is predicting the material
Application be above restricted.
Graphene nano volume is formed by graphene film by helix-coil, is had in unique one-dimensional tube-like condition and opening
Chamber is a kind of new topological structure of grapheme material.Graphene nano, which is rolled up, has both carbon nanotube and the performance of graphene, while by
Open architecture between its both ends and volume layer is easy to the curling package of nano particle.
Invention content
The present invention proposes the preparation side that a kind of combination nano-particle obtains graphene nano volume under fricting shearing effect
Method, this method make graphene obtain nanometer roll, preparation process letter by the effect of fricting shearing under the cooperation of nano-particle
Single, the period is short and at low cost.
Technical solution provided by the invention is：
A kind of preparation method of graphene nano volume, includes the following steps：
Step 1：The preparation of graphene coated nano particle
A) preparation of graphite oxide：Mixed solution is formed by crystalline flake graphite, potassium nitrate and the concentrated sulfuric acid first, according to dense sulphur
Acid, crystalline flake graphite and potassium nitrate sequence sequentially add, and potassium permanganate are then added in above-mentioned solution, and at a temperature of 40 DEG C
It is kept stirring 3 hours；Deionized water is added in solution again, 65-80 DEG C of temperature is heated to, is continued with 800-1000rpm. rotating speeds
20-90min obtains solution A；Hydrogen peroxide is added in deionized water and is uniformly mixing to obtain hydrogenperoxide steam generator, it will be above-mentioned
Prepare obtain solution A be poured slowly into hydrogenperoxide steam generator and stir evenly with sodium hydroxide adjustment pH value be 5-6, obtain molten
Liquid B is centrifuged 30 minutes in the centrifuge of 8000rpm, is obtained liquid and solid separation phase, is recycled ethanol solution centrifugation
8000rpm removes remaining impurity in 25 minutes, obtains graphite oxide；
B) preparation of redox graphene：Graphite oxide after separation is added in into the water that mass percent is 8%-12%
It closes hydrazine reductase 12-4 hours, then add in deionized water and the mixed solution is added in reaction kettle, in 80 DEG C of reactions
800min prepares redox graphene RGO；
C) preparation of graphene coated nano zircite：A certain amount of ZrOCl is taken first2·8H2O powder and deionized water
It is configured to the ZrOCl of 0.3mol/L2Aqueous solution adds in lactic acid into prepared solution, uniform with magnetic stirrer, then
Add in a certain amount of Y (NO3)3Powder and ErCl3Powder, Y in obtained mixed solution3+A concentration of 0.02mol/L, Er3+It is a concentration of
0.08mol/L；It is adjusted with NaOH and mixed solution is transferred to polytetrafluoroethylene (PTFE) after this mixed solution pH value is regulated for 6, pH
In liner, which is placed in reaction kettle and is reacted 24 hours at 160 DEG C；By reaction solution centrifugal sedimentation, with distilled water and nothing
Water-ethanol washs, and through 80 DEG C of drying and processings, obtains Er3+The yttrium of doping stablizes nanometer ZrO2Powder；
D) then the redox graphene RGO ultrasonic disperses for preparing step b) are added in and are prepared in absolute ethyl alcohol
Rare earth mixing with nano Zirconium powder, be 1 with the mass ratio of RGO:1, ultrasonic disperse is uniformly mixed it, obtains RGO packets
Cover the absolute ethyl alcohol dispersion liquid of nano zirconia particles；
Step 2：Fricting shearing method prepares graphene nano volume
The texturing of stainless steel substrate surface laser is handled, by the absolute ethyl alcohol of above-mentioned RGO cladding nano zirconia particles
Dispersion liquid is spun on stainless steel substrate, rotating speed 1000r/min, time 30s, then 80 DEG C of bakings in vacuum drying chamber
It is dry, by dried stainless steel substrates as on frictional testing machine, 6mmSi3N4Abrading-ball, load 100g, 200r/min, rub 20-
30min, by gained abrasive dust ultrasonic disperse in absolute ethyl alcohol, gained is the dispersion liquid of graphene nano volume.
In step a), being added in every 100ml solution As has the crystalline flake graphite of 1.0-2.0g, the potassium nitrate of 2.0-2.5,4.5-
The potassium permanganate of 6.5g.
In step a), in hydrogenperoxide steam generator, the volume ratio of hydrogen peroxide and deionized water is 1:20；Solution A and peroxide
The volume ratio for changing hydrogen solution is 1:4.
In step b), 0.1-0.2g graphite oxides are added in the deionized water per 25-35ml.
In step c), ZrOCl2The volume ratio of aqueous solution and lactic acid is 24:5.
In step d), the mass/volume ratio of redox graphene and absolute ethyl alcohol is 1:100g/ml.
The texturing of stainless steel substrate surface laser is handled：The stainless steel substrates of 15mm × 15mm are taken, polishes, throw by surface
After light and cleaning treatment, in steel disc surface ND：The pulse laser of YAG20kHz carries out laser boring, each hole it is a diameter of
150 μm, the two neighboring aperture center of circle is at a distance of 500 μm, i.e. two the edge of the circles are at a distance of 350 μm.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention provides a kind of method that graphene nano volume is prepared by fricting shearing method, with reduction-oxidation graphite obtained
Alkene is raw material, and under the driving of nano zirconia particles, large stretch of graphene bending is coated.Under the action of fricting shearing,
Large stretch of graphene of buckle fold, which is constantly sheared, to become smaller, and further curl into nanometer roll.It can after ultrasonic disperse
So that nanometer roll is detached with nano-particle.
The present invention has the material and shape of nano-particle a larger selectivity, obtained nanometer roll and nano-particle
Separation is also relatively easy to.And the preparation process of this method is simple, and the period is short and at low cost.
Description of the drawings
Fig. 1 is the Raman collection of illustrative plates (excitation wavelength of graphene and abrasive dust before and after the friction of nano zirconia particles laminated film
514nm)。
Fig. 2 is the TEM figures of graphene nano volume.
Specific embodiment
With reference to specific embodiment, the invention will be further described.
Step 1：The preparation of graphene coated nano particle
The preparation of graphite oxide：First by the crystalline flake graphite that mass percent is 1.0-2.0g, the potassium nitrate of 2.0-2.5 with
And remaining concentrated sulfuric acid composition mixed solution, it is sequentially added according to the concentrated sulfuric acid, crystalline flake graphite and potassium nitrate sequence, then above-mentioned
The potassium permanganate of 4.5-6.5g is added in solution, and is kept stirring at a temperature of 40 DEG C 3 hours；Deionized water is added in again molten
To 100ml in liquid, and 65-80 DEG C of temperature is heated to, 20-90min is continued with 800-1000rpm. rotating speeds；By 20ml hydrogen peroxide
It is added in 400ml deionized waters and stirs evenly, the solution of above-mentioned preparation is poured slowly into hydrogenperoxide steam generator and stirs
It is even.It is 5-6 with sodium hydroxide adjustment pH value, is centrifuged 30 minutes in the centrifuge of 8000rpm, obtains liquid and solid separation
Phase recycles ethanol solution centrifugation 8000rpm to remove remaining impurity in 25 minutes, obtains graphite oxide；
The preparation of redox graphene：It is 8%- that 0.1-0.2g graphite oxides after separation are added in mass percent
Then 12% hydrazine hydrate reduction 2-4 hours adds in the deionized water of 25-35ml and the mixed solution is added to reaction kettle
In, 800min is reacted at 80 DEG C, prepares redox graphene；The preparation of graphene coated nano zircite：One is taken first
Quantitative ZrOCl2·8H2O powder is configured to the ZrOCl of the 24ml of 0.3mol/L with deionized water2Aqueous solution, to prepared
The lactic acid of 5ml is added in solution, it is uniform with magnetic stirrer, add a certain amount of Y (NO3)3Powder and ErCl3Powder obtains
To mixed solution in Y3+A concentration of 0.02mol/L, Er3+A concentration of 0.08mol/L；This mixed solution pH value is adjusted with NaOH
Mixed solution is transferred in polytetrafluoroethyllining lining after being regulated for 6, pH, which is placed in reaction kettle at 160 DEG C
Lower reaction 24 hours；It by reaction solution centrifugal sedimentation, is washed with distilled water and absolute ethyl alcohol, through 80 DEG C of drying and processings, obtains Er3+It mixes
Miscellaneous yttrium stablizes nanometer ZrO2Powder；
By the RGO0.08-0.12g ultrasonic disperses of above-mentioned preparation in the absolute ethyl alcohol of 8-12ml, then add in and prepare
Rare earth mixing with nano Zirconium powder, be 1 with the mass ratio of RGO:1, ultrasonic disperse is uniformly mixed it, obtains RGO packets
Cover the absolute ethyl alcohol dispersion liquid of nano zirconia particles；
Step 2：Fricting shearing method prepares graphene nano volume
The texturing of stainless steel substrate surface laser is handled：The stainless steel substrates of 15mm × 15mm are taken, polishes, polish by surface
After cleaning treatment, in steel disc surface ND：The pulse laser of YAG20kHz carries out laser boring, each hole it is a diameter of
150 μm, the two neighboring aperture center of circle is at a distance of 500 μm, i.e. two the edge of the circles are at a distance of 350 μm；
The absolute ethyl alcohol dispersion liquid of above-mentioned RGO cladding nano zirconia particles is spun on stainless steel substrate, rotating speed is
1000r/min, time 30s, then 80 DEG C of drying in vacuum drying chamber, by dried stainless steel substrates as friction test
On machine, 6mmSi3N4Abrading-ball, load 100g, 200r/min, rub 20-30min, by gained abrasive dust ultrasonic disperse in absolute ethyl alcohol
In, gained is the dispersion liquid of graphene nano volume.
Fig. 1 is the Raman collection of illustrative plates (excitation wavelength of graphene and abrasive dust before and after the friction of nano zirconia particles laminated film
514nm).It can be found that ZrO from figure2Raman spectra from the 634cm before friction-1The 642cm being moved to after friction-1.
1344cm-1With 1598cm-1There is the characteristic peak D peaks of graphene and G peaks respectively in place.ID/IGIt is changed to from 0.97 before friction
0.83 after friction.
Fig. 2 is the TEM figures of graphene nano volume.Many graphene nano volumes as can be observed from Figure, with carbon nanotube
Structure it is quite similar.
The above is only presently preferred embodiments of the present invention, not makees limitation in any form to the present invention, any ripe
Professional and technical personnel is known, without departing from the scope of the present invention, technical spirit according to the present invention, to above real
Apply any simple modification, equivalent replacement that example made and improve etc., still fall within technical solution of the present invention protection domain it
It is interior.
Claims (7)
1. a kind of preparation method of graphene nano volume, it is characterised in that：Include the following steps：
Step 1：The preparation of graphene coated nano particle
A) preparation of graphite oxide：Mixed solution is formed by crystalline flake graphite, potassium nitrate and the concentrated sulfuric acid first, according to the concentrated sulfuric acid,
Crystalline flake graphite and potassium nitrate sequence sequentially add, and potassium permanganate are then added in above-mentioned solution, and protected at a temperature of 40 DEG C
Hold stirring 3 hours；Deionized water is added in solution again, 65-80 DEG C of temperature is heated to, is continued with 800-1000rpm. rotating speeds
20-90min obtains solution A；Hydrogen peroxide is added in deionized water and is uniformly mixing to obtain hydrogenperoxide steam generator, it will be above-mentioned
Prepare obtain solution A be poured slowly into hydrogenperoxide steam generator and stir evenly with sodium hydroxide adjustment pH value be 5-6, obtain molten
Liquid B is centrifuged 30 minutes in the centrifuge of 8000rpm, is obtained liquid and solid separation phase, is recycled ethanol solution centrifugation
8000rpm removes remaining impurity in 25 minutes, obtains graphite oxide；
B) preparation of redox graphene：Graphite oxide after separation is added in into the hydrazine hydrate that mass percent is 8%-12%
Then reductase 12-4 hours adds in deionized water and the mixed solution is added in reaction kettle, 800min, system are reacted at 80 DEG C
It is standby go out redox graphene RGO；
C) preparation of graphene coated nano zircite：A certain amount of ZrOCl is taken first2·8H2O powder is prepared with deionized water
Into the ZrOCl of 0.3mol/L2Aqueous solution adds in lactic acid into prepared solution, uniform with magnetic stirrer, adds
A certain amount of Y (NO3)3Powder and ErCl3Powder, Y in obtained mixed solution3+A concentration of 0.02mol/L, Er3+It is a concentration of
0.08mol/L；It is adjusted with NaOH and mixed solution is transferred to polytetrafluoroethylene (PTFE) after this mixed solution pH value is regulated for 6, pH
In liner, which is placed in reaction kettle and is reacted 24 hours at 160 DEG C；By reaction solution centrifugal sedimentation, with distilled water and nothing
Water-ethanol washs, and through 80 DEG C of drying and processings, obtains Er3+The yttrium of doping stablizes nanometer ZrO2Powder；
D) by step b) prepare redox graphene RGO ultrasonic disperses in absolute ethyl alcohol, then add in prepare it is dilute
Native doped nano zirconia powder, the mass ratio with RGO are 1:1, ultrasonic disperse is uniformly mixed it, obtains RGO claddings and receives
The absolute ethyl alcohol dispersion liquid of rice Zirconia particles；
Step 2：Fricting shearing method prepares graphene nano volume
The texturing of stainless steel substrate surface laser is handled, the absolute ethyl alcohol of above-mentioned RGO cladding nano zirconia particles is disperseed
Liquid is spun on stainless steel substrate, rotating speed 1000r/min, time 30s, then 80 DEG C of drying in vacuum drying chamber, will
Dried stainless steel substrates are as on frictional testing machine, 6mmSi3N4Abrading-ball, load 100g, 200r/min, rub 20-30min,
By gained abrasive dust ultrasonic disperse in absolute ethyl alcohol, gained is the dispersion liquid of graphene nano volume.
2. the preparation method of graphene nano volume according to claim 1, it is characterised in that：It is molten per 100ml in step a)
The potassium permanganate for having the crystalline flake graphite of 1.0-2.0g, the potassium nitrate of 2.0-2.5,4.5-6.5g is added in liquid A.
3. the preparation method of graphene nano volume according to claim 1, it is characterised in that：In step a), hydrogen peroxide
In solution, the volume ratio of hydrogen peroxide and deionized water is 1:20；Solution A and the volume ratio of hydrogenperoxide steam generator are 1:4.
4. the preparation method of graphene nano volume according to claim 1, it is characterised in that：In step b), per 25-35ml
Deionized water in add in 0.1-0.2g graphite oxides.
5. the preparation method of graphene nano volume according to claim 1, it is characterised in that：In step c), ZrOCl2It is water-soluble
The volume ratio of liquid and lactic acid is 24:5.
6. the preparation method of graphene nano volume according to claim 1, it is characterised in that：In step d), reduction-oxidation
The mass/volume of graphene and absolute ethyl alcohol ratio is 1:100g/ml.
7. the preparation method of graphene nano volume according to claim 1, it is characterised in that：Stainless steel substrate surface laser
Texturing is handled：Take the stainless steel substrates of 15mm × 15mm, polish by surface, polish and cleaning treatment after, on steel disc surface
Use ND：The pulse laser progress laser boring of YAG20kHz, a diameter of 150 μm of each hole, two neighboring aperture center of circle phase
Away from 500 μm, i.e. two the edge of the circles are at a distance of 350 μm.
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Cited By (6)
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| CN109505117A (en) * | 2018-09-19 | 2019-03-22 | 南京信息工程大学 | A kind of composite modifying method of porous fibrous structure |
| CN110396838A (en) * | 2019-07-19 | 2019-11-01 | 浙江海印数码科技有限公司 | Modified ink-jet printed use coating type ink of a kind of compound particle based on multilevel structure and preparation method thereof, application |
| CN113311045A (en) * | 2021-07-16 | 2021-08-27 | 福建师范大学 | Preparation method of graphene nano-roll cured clenbuterol hydrochloride sensor |
| CN113880079A (en) * | 2021-11-12 | 2022-01-04 | 四川大学 | Graphene nano-roll and preparation method thereof |
| CN114142076A (en) * | 2021-11-30 | 2022-03-04 | 成都先进金属材料产业技术研究院股份有限公司 | Method for improving electrochemical activity of vanadium battery electrolyte |
| CN114142076B (en) * | 2021-11-30 | 2024-04-19 | 成都先进金属材料产业技术研究院股份有限公司 | Method for improving electrochemical activity of vanadium battery electrolyte |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109505117A (en) * | 2018-09-19 | 2019-03-22 | 南京信息工程大学 | A kind of composite modifying method of porous fibrous structure |
| CN110396838A (en) * | 2019-07-19 | 2019-11-01 | 浙江海印数码科技有限公司 | Modified ink-jet printed use coating type ink of a kind of compound particle based on multilevel structure and preparation method thereof, application |
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| CN113311045A (en) * | 2021-07-16 | 2021-08-27 | 福建师范大学 | Preparation method of graphene nano-roll cured clenbuterol hydrochloride sensor |
| CN113880079A (en) * | 2021-11-12 | 2022-01-04 | 四川大学 | Graphene nano-roll and preparation method thereof |
| CN114142076A (en) * | 2021-11-30 | 2022-03-04 | 成都先进金属材料产业技术研究院股份有限公司 | Method for improving electrochemical activity of vanadium battery electrolyte |
| CN114142076B (en) * | 2021-11-30 | 2024-04-19 | 成都先进金属材料产业技术研究院股份有限公司 | Method for improving electrochemical activity of vanadium battery electrolyte |
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Application publication date: 20180619 |