CN108314029B - Hollow bowl-shape graphene oxide micro motor and preparation method thereof - Google Patents
Hollow bowl-shape graphene oxide micro motor and preparation method thereof Download PDFInfo
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- CN108314029B CN108314029B CN201810047672.6A CN201810047672A CN108314029B CN 108314029 B CN108314029 B CN 108314029B CN 201810047672 A CN201810047672 A CN 201810047672A CN 108314029 B CN108314029 B CN 108314029B
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Abstract
The invention discloses a kind of hollow bowl-shape graphene oxide micro motors and preparation method thereof, and hollow bowl-shape graphene oxide micro motor is the asymmetric three-dimensional hollow bowl structure of 30 μm ~ 1.5mm of diameter.At room temperature, shearing force is provided just with 50 ~ 2800 r/min of electric blender, the capillarity generated in conjunction with drying at room temperature, without freeze-drying, soft template or sacrifice hard template, it is easy to operate, it is low in cost, size is controllable, it is applicable to large-scale industrial production.Prepared hollow bowl-shape graphene oxide micro motor is put into the hydrogenperoxide steam generator that mass percent concentration is 5%, oxygen is generated by catalyzing hydrogen peroxide, self-propelled campaign is realized using oxygen bubble as power, and realize that the simple recycling of micro motor and magnetic field control using hollow bowl-shape graphene oxide micro motor magnetic properties, to achieve the purpose that the positioning operation in the solution containing hydrogen peroxide.
Description
Technical field
The present invention relates to a kind of artificial micro motor and preparation method thereof, providing a kind of easy to operate, low in cost, size can
Control and the hollow bowl-shape graphene oxide micro motor suitable for large-scale industrial production and preparation method thereof.
Background technique
Artificial micro motor is that one kind can convert having for motion energy for chemical energy, luminous energy, the electric energy etc. in environment
From the micro-nano functional material of drive characteristic, for stock size in nanoscale to micron order, Typical Representative is Janus particle and pipe
Decline motor (Angew. Chem. Int. Ed. 2014,53,2).Several typical building methods are had been developed that at present,
As electrochemical deposition (Small 2015,11,499), physical vapour deposition (PVD) (ACS Nano 2012,6,8432) and film roll are bent
Technology (Chem. Soc. Rev. 2011,40,2109) etc..But existing building method is related to more complex step mostly,
The production equipment of some valuableness is needed, large-scale industrial production is difficult to realize.
Graphene oxide (Graphene oxide, GO) is the important presoma for preparing graphene, and surface exists a large amount of
sp2The functional groups such as the carbon structure unit and hydroxyl (- OH) of hydridization, alkoxy (C-O-C), carboxyl (- COOH) and carbonyl (C=O).
GO has so excellent structural property, be widely used to three-dimensional grapheme and graphene oxide macroscopic material construct and
The fields such as catalysis, the energy, environment show brilliant contribution.It is reported according to existing literature, prepares graphene macroscopic material at present
Frequently with template CVD method (Small 2011,7,3163;Sci. Rep. 2013,3,2125) and hydro-thermal method (ACS
Nano, 2010, 4, 4324; Adv. Mater. 2012, 24, 5124; Sci. Rep. 2013, 3, 2975;
Adv. Mater. 2014, 26, 4789; J. Phys. Chem. C 2015, 119, 24373).Wherein, template CVD method
It is generally necessary to which sacrificing template obtains porous three-dimensional structure, experimental implementation is complicated, and increases operating cost；Hydro-thermal method is using in advance
The graphene hydrogel first prepared removes the solvent in hydrogel in conjunction with Freeze Drying Technique or air drying technology
The graphene macroform with three-dimensional net structure is obtained, however often with the reduction of GO during hydro-thermal method self assembly,
Surface oxygen functional group is caused to reduce (Nanoscale 2012,4,5549).It is bent other than above two self-assembling method
Liang Ti seminar et al. is coupler using aniline, prepares three-dimensional GO material (Adv. Mater. using room temperature self-assembly method
2016,28,10287), gained macrostructure structure is closely knit and diameter is up to several centimeters, symmetrical structure and biggish close
Degree, limits its practical application as micro motor.
Hollow sphere or hollow bowl-shape carbon-based material are generally prepared using soft template (emulsion method) or hard template method at present.Such as
Zheng Yuan etc. prepares the polyaniline-graphite alkene tiny balloon having a size of 25 μm or so using Pickering emulsion method, and this method needs
To the auxiliary (chemical journal, 2017,75,391) of the preparatory sulfonation modifying of graphene and microemulsion.Ding Shujiang etc. uses polystyrene
Microballoon is template, prepares the hollow bowl-shape carbon based metal oxide composite (number of patent application of various compositions
CN201410406726.5).
Summary of the invention
The present invention is provided a kind of easy to operate, at low cost to solve above-mentioned technical problem present in the prior art
Honest and clean, size is controllable and the hollow bowl-shape graphene oxide micro motor suitable for large-scale industrial production and preparation method thereof.
The technical solution of the invention is as follows: a kind of hollow bowl-shape graphene oxide micro motor, it is characterized in that asymmetry three
Hollow bowl structure is tieed up, average diameter is 30 μm ~ 1.5 mm.
A kind of preparation method of above-mentioned hollow bowl-shape graphene oxide micro motor carries out in accordance with the following steps:
A. graphene oxide is prepared, prepared by the method that the prior art can be used；
B. at room temperature, the suspended of 2 ~ 10 mg/mL is made into water in prepared graphene oxide ultrasonic disperse
Liquid；Then MnFe is added into suspension2O4Powder is ultrasonically formed uniform suspension, the suspension and MnFe2O4Powder
Ratio is the mg of 10 mL:5 ~ 80；Aniline solution is added dropwise again, additional amount is that 200 mL of μ L ~ 5 are added in every 10 mL suspension；
4 ~ 36h finally is stirred with the electric mixer that revolving speed is 50 ~ 2800 r/min, mixed system becomes cotton-shaped heavy by uniform suspension
It forms sediment, centrifugation recycling precipitating, gained is precipitated as the three-dimensional globular macroscopic body of 300 μm ~ 1.5 cm of diameter；
C. after drying at room temperature precipitates for 24 hours, the asymmetric three-dimensional hollow bowl structure that diameter is 30 μm ~ 1.5 mm is obtained.
The graphene oxide for preparing carries out in accordance with the following steps:
1g graphite is added in the concentrated sulfuric acid that 23mL mass percent concentration is 98%, ice bath cooling lower stirring 2 hours, is delayed
It is slow that 3g potassium permanganate is added, continue stirring 2 hours in the cooling condition, then mixture is transferred in 35 DEG C of water-baths and reacts 1
Hour, then it is slowly added to the distilled water of 58 mL thereto, bath temperature is risen to 98 DEG C after mixing evenly, is stirred 1 hour；From
The beaker for filling mixture is taken out in water-bath, the warm water of 60 DEG C of 140 mL is slowly added under stirring condition, and under agitation
It is cooled to 25 DEG C；The hydrogen peroxide that 5 mL mass percent concentrations are 30% is added into mixture, obtains oxygen after mixing evenly
Graphite alkene suspension, finally by suspension centrifuge washing to neutrality, 80 DEG C of dryings.Dosage in actual production between each reactant
It can be carried out according to aforementioned proportion.
The present invention makes full use of the cooperation mechanism of shearing force and capillarity, using electric stirring and air drying technology,
Can directly preparation structure be 30 μm ~ 1.5 mm of diameter asymmetric three-dimensional hollow bowl structure graphene oxide micro motor,
Without freeze-drying, soft template (microemulsion) or hard template is sacrificed, it is easy to operate, it is low in cost, size is controllable, it is applicable to
Large-scale industrial production.Prepared hollow bowl-shape graphene oxide micro motor is put into the peroxide that mass percent concentration is 5%
Change in hydrogen solution, oxygen is generated by catalyzing hydrogen peroxide, realizes self-propelled campaign using oxygen bubble as power, and utilize
Hollow bowl-shape graphene oxide micro motor magnetic properties realize the simple recycling and magnetic field control of micro motor, are containing to reach
The purpose of positioning operation in the solution of hydrogen peroxide.
Detailed description of the invention
Fig. 1 is the process flow chart of preparation method of the embodiment of the present invention.
Fig. 2 is the XRD spectra of hollow bowl-shape graphene oxide micro motor in the embodiment of the present invention 1.
Fig. 3 is the stereoscan photograph of hollow bowl-shape graphene oxide micro motor in the embodiment of the present invention 1.
Fig. 4 is the stereoscan photograph of hollow bowl-shape graphene oxide micro motor in the embodiment of the present invention 2.
Specific embodiment
Embodiment 1:
A kind of preparation method of above-mentioned hollow bowl-shape graphene oxide micro motor carries out in accordance with the following steps as shown in Figure 1:
A. graphene oxide is prepared:
1g graphite is added in the concentrated sulfuric acid that 23 mL mass percent concentrations are 98%, ice bath cooling lower stirring 2 hours, is delayed
It is slow that 3g potassium permanganate is added, continue stirring 2 hours in the cooling condition, then mixture is transferred in 35 DEG C of water-baths and reacts 1
Hour, then it is slowly added to the distilled water of 58 mL thereto, bath temperature is risen to 98 DEG C after mixing evenly, is stirred 1 hour；From
The beaker for filling mixture is taken out in water-bath, the warm water of 60 DEG C of 140 mL is slowly added under stirring condition, and under agitation
It is cooled to 25 DEG C；To mixture (graphite oxide, SO4、K+、Mn2+And H+) in 5 mL mass percent concentrations are added is 30%
Hydrogen peroxide obtains graphene oxide suspension after mixing evenly, finally by suspension centrifuge washing to neutrality, 80 DEG C of dryings；
B. under room temperature (15-30 DEG C), by prepared graphene oxide ultrasonic disperse into water, 10 mg/mL are made
Suspension；Then 10 mL suspensions are taken, 40 mg MnFe are added thereto2O4Powder is ultrasonically formed uniform suspension；Again by
It is added dropwise to 5 mL aniline solutions；36h finally is stirred with the electric mixer that revolving speed is 50 r/min, mixed system is by uniform suspended
Liquid becomes flocculent deposit, centrifugation recycling precipitating, and gained is precipitated as wet three-dimensional globular macroscopic body；
C. after (15-30 DEG C) drying for 24 hours of room temperature, asymmetric three-dimensional hollow bowl structure is obtained, i.e., hollow bowl-shape oxidation stone
Black alkene micro motor.
The average diameter of the three-dimensional globular macroscopic body of the obtained moisture state of b step is 1.5 cm, under the state
Macroscopic body have good ductility, macrostructure of different shapes can be molded.When the three-dimensional globular of moisture state
Macroscopic body is after step c is dry, and with scanning electron microscopic observation, its surface texture shows asymmetric three-dimensional hollow bowl structure, average
Diameter is contracted to 1.5 mm.
The XRD spectra and stereoscan photograph difference of the 1 hollow bowl-shape graphene oxide micro motor of gained of the embodiment of the present invention
As shown in Figure 2 and Figure 3.A in Fig. 3 is the scanning electron microscope (SEM) photograph that the micro motor of preparation is shown from " the rim of a bowl " direction；B is in figure a box
Partial enlarged drawing.
Embodiment 2:
Preparation method is substantially with embodiment 1, the difference is that the dilute turbid liquid concentration of graphite oxide is diluted to 2 in b step
5 mg MnFe are added in mg/mL2O4Powder, ultrasound forms uniform suspension in 15 minutes, then 200 μ L aniline are added dropwise, electronic
After blender stirs 4h under 2800 r/min speed conditions, recycling precipitating.
Wherein the average diameter of moisture state macroscopic body is 300 μm, and asymmetric hollow bowl structure is showed after dry, is put down
Equal diameter is contracted to 30 μm or so.The stereoscan photograph of the 2 hollow bowl-shape graphene oxide micro motor of gained of the embodiment of the present invention
As shown in Figure 4.
Embodiment 3:
Preparation method is substantially with embodiment 1, the difference is that being turned using electric mixer in 1000 r/min in b step
Precipitating is recycled after stirring 36h under the conditions of speed.
Wherein the average diameter of the macroscopic body of moisture state is 3 mm, and asymmetric hollow bowl structure is showed after dry, is put down
Equal diameter is contracted to 300 μm.
Embodiment 4:
Preparation method is substantially with embodiment 1, the difference is that 80 mg MnFe are added in b step2O4Powder, electric mixing
It mixes after device stirs 36h under 1000 r/min speed conditions and recycles precipitating.
Wherein the average diameter of moisture state macroscopic body is 1.5 mm, and asymmetric hollow bowl structure is showed after dry, is put down
Equal diameter is contracted to 150 μm.
Claims (2)
1. a kind of preparation method of hollow bowl-shape graphene oxide micro motor, the hollow bowl-shape graphene oxide micro motor is not
The hollow bowl structure of symmetric three-dimensional, average diameter are 30 μm ~ 1.5 mm；It is characterized in that carrying out in accordance with the following steps:
A. graphene oxide is prepared；
B. at room temperature, the suspension of 2 ~ 10 mg/mL is made into water in prepared graphene oxide ultrasonic disperse；So
MnFe is added in backward suspension2O4Powder is ultrasonically formed uniform suspension, the suspension and MnFe2O4The ratio of powder is
The mg of 10 mL:5 ~ 80；Aniline solution is added dropwise again, additional amount is that 200 mL of μ L ~ 5 are added in every 10 mL suspension；Finally use
Revolving speed, which stirs for the electric mixer of 50 ~ 2800 r/min to mixed system, becomes flocculent deposit by uniform suspension, and recycling is heavy
It forms sediment；
C. drying at room temperature precipitates, and obtains the asymmetric three-dimensional hollow bowl structure graphene oxide that diameter is 30 μm ~ 1.5 mm
Micro motor.
2. the preparation method of hollow bowl-shape graphene oxide micro motor according to claim 1, it is characterised in that the preparation
Graphene oxide carries out in accordance with the following steps:
1g graphite is added to 23 mL mass percent concentrations as in 98% concentrated sulfuric acid, the cooling lower stirring of ice bath 2 hours slowly adds
Enter 3g potassium permanganate, continue stirring 2 hours in the cooling condition, then mixture is transferred in 35 DEG C of water-baths and is reacted 1 hour,
It is slowly added to the distilled water of 58 mL thereto again, bath temperature is risen to 98 DEG C after mixing evenly, stir 1 hour；From water-bath
The beaker for filling mixture is taken out, is slowly added to the warm water of 60 DEG C of 140 mL under stirring condition, and be cooled under agitation
25℃；The hydrogen peroxide that 5 mL mass percent concentrations are 30% is added into mixture, obtains graphite oxide after mixing evenly
Alkene suspension, finally by suspension centrifuge washing to neutrality, 80 DEG C of dryings.
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Citations (4)
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| CN103121672A (en) * | 2013-03-20 | 2013-05-29 | 中国科学院苏州纳米技术与纳米仿生研究所 | Graphene oxide microsphere and graphene microsphere and preparation methods thereof |
| KR20140118064A (en) * | 2013-03-28 | 2014-10-08 | 한국지질자원연구원 | Manufacturing method for graphene hollow particle and graphene hollow particle using the same |
| CN105331999A (en) * | 2015-10-13 | 2016-02-17 | 湖南农业大学 | Preparing method for hollow graphene |
| CN106129373A (en) * | 2016-08-25 | 2016-11-16 | 陕西科技大学 | A kind of hollow ball Fe2o3the preparation method of/rGO lithium ion battery negative material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103121672A (en) * | 2013-03-20 | 2013-05-29 | 中国科学院苏州纳米技术与纳米仿生研究所 | Graphene oxide microsphere and graphene microsphere and preparation methods thereof |
| KR20140118064A (en) * | 2013-03-28 | 2014-10-08 | 한국지질자원연구원 | Manufacturing method for graphene hollow particle and graphene hollow particle using the same |
| CN105331999A (en) * | 2015-10-13 | 2016-02-17 | 湖南农业大学 | Preparing method for hollow graphene |
| CN106129373A (en) * | 2016-08-25 | 2016-11-16 | 陕西科技大学 | A kind of hollow ball Fe2o3the preparation method of/rGO lithium ion battery negative material |
Non-Patent Citations (2)
| Title |
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| Graphene-Based Microbots for Toxic Heavy Metal Removal and Recovery from Water;Diana Vilela et al.;《Nano Lett.》;20160321;第16卷;第2860-2866页 |
| Self-Propelled Micro/Nanoparticle Motors;Maria Guix et al.;《Part. Part. Syst. Charact.》;20180115;第35卷;第1-31页 |
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Application publication date: 20180724 Assignee: Yangjiang jiyoulan Electronic Technology Co.,Ltd. Assignor: DONGGUAN University OF TECHNOLOGY Contract record no.: X2022980027700 Denomination of invention: Hollow bowl-shaped graphene oxide micromotor and its preparation method Granted publication date: 20190312 License type: Common License Record date: 20221230 |
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Application publication date: 20180724 Assignee: Guangdong Meisong New Material Co.,Ltd. Assignor: DONGGUAN University OF TECHNOLOGY Contract record no.: X2023980030287 Denomination of invention: Hollow bowl-shaped graphene oxide micromotor and its preparation method Granted publication date: 20190312 License type: Common License Record date: 20230110 |