CN105293481A - Method for ultrasonically cutting graphene oxide - Google Patents
Method for ultrasonically cutting graphene oxide Download PDFInfo
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- CN105293481A CN105293481A CN201510881904.4A CN201510881904A CN105293481A CN 105293481 A CN105293481 A CN 105293481A CN 201510881904 A CN201510881904 A CN 201510881904A CN 105293481 A CN105293481 A CN 105293481A
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Abstract
The invention discloses a method for ultrasonically cutting graphene oxide. The method comprises the following steps: step I, adding the graphene oxide into water to obtain a graphene oxide suspension; step II, treating the graphene oxide suspension in the step I by virtue of an ultrasonic device, and controlling the temperature of the graphene oxide suspension at a range of 30 to 50 DEG C; step III, centrifuging the graphene oxide suspension in the step II to obtain the graphene oxide precipitates; step IV, drying the graphene oxide precipitates in the step III to obtain the nano graphene sheets. The method for ultrasonically cutting the graphene oxide is moderate in cutting condition, and no other chemical substance is added; moreover, the method is easy to implement and low in cost, and the prepared nano graphene oxide sheets are small in size and narrow in distribution. The diameter of the prepared nano oxide graphite sheet is reduced to 220n to 370nm; moreover, the oxidation degree of the graphene oxide is not obviously different from that of the raw material.
Description
Technical field
The present invention relates to grapheme material technical field, be specifically related to a kind of method of ultrasonic cutting graphene oxide.
Background technology
Graphene oxide is a kind of thin layer of monatomic thickness, is desirable two-dimension nano materials.Graphene oxide has excellent mechanical property and good thermostability.In addition, surface of graphene oxide contains a large amount of functional groups, thus in water, has good dispersing property, and can carry out chemically modified.Therefore, graphene oxide is widely used in fields such as functional composite material, coating, ink, biological medicines.
Graphene oxide is generally obtained by chemical processes such as Brodie method, Staudenmaier method or Hummers methods, and gained lamella diameter is generally in micron level.When graphene oxide is in field application such as functional composite materials, particularly when preparing ultra-thin composite separating film, require that the diameter of graphene oxide is at below 500nm.Therefore, need graphene oxide cutting to reduce its lamella size.
At present, the method for cutting out of graphene oxide mainly comprises acidifying cutting and hydro-thermal cutting, and these two kinds of methods all exist drawback.Acidifying cutting process need adds strong acid, and use procedure is dangerous, and this process is large to equipment corrosion, and operation easier is large.Hydro-thermal cutting process is carried out under high-temperature and high-pressure conditions, and operation easier is large, dangerous large.Therefore, current method of cutting out condition is harsh, and high to equipment requirements, cost is higher.
Summary of the invention
Instant invention overcomes the deficiencies in the prior art, provide the Graphene method of cutting out of a kind of mild condition, easy and simple to handle, economical and efficient, and the method can not affect the degree of oxidation of graphene oxide.
The graphene oxide that the present invention adopts chemical method to prepare is raw material, adopts ultrasonicly to carry out cutting, significantly reduces the lamella size of graphene oxide, and does not change its degree of oxidation.Method of the present invention relative to traditional graphene oxide cutting technique, safer, environmental protection, efficient, easy suitability for industrialized production.
For solving above-mentioned technical problem, the present invention by the following technical solutions:
A method for ultrasonic cutting graphene oxide, described method comprises the following steps:
Step one: be added to the water by graphene oxide, obtains graphene oxide suspension;
Step 2: by the ultrasonic device process of graphene oxide suspension in step one, controls described graphene oxide suspension temperature within the scope of 30 DEG C ~ 50 DEG C;
Step 3: graphene oxide suspension in step 2 is carried out centrifugal treating, obtains graphene oxide precipitation;
Step 4: by dry for the precipitation of graphene oxide described in step 3, obtain nano graphene oxide sheet.
Further technical scheme is that graphene oxide in step one is obtained by Brodie method, Staudenmaier method or Hummers method, and described graphene oxide lamella diameter is 1000 ~ 5000nm.
Further technical scheme is that in step 2, ultrasonic power is 300w ~ 900w, and ultrasonic time is 1h ~ 10h.
Further technical scheme is that in step 2, graphene oxide suspension temperature adopts water-bath to control.
Further technical scheme is that in step 3, centrifugation rate is 10000r/min ~ 15000r/min, and centrifugation time is 0.5h ~ 2h.
Further technical scheme is that in step 4, drying mode comprises and adopts vacuum drying oven dry or adopt and revolve that to steam instrument dry, and drying temperature is 50 DEG C, and time of drying is 2 hours.
Further technical scheme is the lamella diameter of nano graphene oxide sheet is 220 ~ 370nm.
Further technical scheme is that the degree of oxidation of nano graphene oxide sheet is consistent with the degree of oxidation of described graphene oxide.
Compared with prior art, the invention has the beneficial effects as follows: the method cutting mild condition of ultrasonic cutting graphene oxide of the present invention, do not add other chemical substances, therefore easy to implement, cost is low, the little and narrowly distributing of obtained nano graphene oxide chip size.The diameter of obtained nano graphene oxide sheet is reduced to 220 ~ 370nm, and the degree of oxidation of graphene oxide no significant difference compared with raw material.
Accompanying drawing explanation
Fig. 1 is the nano graphene oxide of one embodiment of the invention and the ultraviolet-visible absorption spectroscopy figure of graphene oxide raw material.
Fig. 2 is the nano graphene oxide atomic force microscope figure (AFM) of one embodiment of the invention.
Fig. 3 is the atomic force microscope figure (AFM) of the graphene oxide raw material of one embodiment of the invention.
Fig. 4 is the nano graphene oxide of one embodiment of the invention and the infrared absorpting light spectra (FTIR) of graphene oxide raw material.
Fig. 5 is the nano graphene oxide of one embodiment of the invention and the thermal weight loss spectrogram (TGA) of graphene oxide raw material.
Embodiment
All features disclosed in this specification sheets, or the step in disclosed all methods or process, except mutually exclusive feature and/or step, all can combine by any way.
Arbitrary feature disclosed in this specification sheets (comprising any accessory claim, summary and accompanying drawing), unless specifically stated otherwise, all can be replaced by other equivalences or the alternative features with similar object.That is, unless specifically stated otherwise, each feature is an example in a series of equivalence or similar characteristics.
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in detail.
Embodiment 1
0.5g graphene oxide raw material is added in 500mL water, at room temperature uses power 300W ultrasonic disperse 30 minutes, obtain finely dispersed suspension.Use power 600w supersound process suspension 7 hours, period controls solution temperature within the scope of 30 DEG C ~ 50 DEG C with water-bath.By the suspension after process be under the condition of 15000r/min centrifugal 30 minutes at centrifugation rate.By the centrifugal precipitation obtained 50 DEG C of vacuum-dryings 2 hours, obtain nano graphene oxide.Adopt the dispersion liquid of ultraviolet-visible pectrophotometer to nano graphene oxide and graphene oxide raw material to characterize, see accompanying drawing 1.Result shows, cutting rear oxidation Graphene is moved to 225nm place in the displacement of the specific extinction position of 227nm, illustrates that graphene oxide lamella size diminishes.Adopt atomic force microscope test nano graphene oxide and graphene oxide raw material, see accompanying drawing 2 and Fig. 3.Result shows, the mean thickness of graphene oxide raw material is 1.90 ± 0.12nm, and mean diameter is 2520 ± 370nm; Nano graphene oxide mean thickness after cutting is 1.80 ± 0.14nm, and mean diameter is 308 ± 19nm.These results suggest that, through ultrasonic cutting, the size of graphene oxide lamella declines to a great extent, and is still single layer structure.Adopt infrared spectra (FTIR) to characterize nano graphene oxide and graphene oxide raw material, see accompanying drawing 4.The infrared spectrum of two kinds of graphene oxides does not have notable difference, illustrates that cutting process does not cause remarkably influenced to surface of graphene oxide functional group kind and content.Adopt thermogravimetric analyzer (TGA) to characterize nano graphene oxide and graphene oxide raw material, see accompanying drawing 5.The thermal weight loss spectrogram of two kinds of graphene oxides does not have notable difference, illustrates that cutting process does not cause remarkably influenced to the chemical constitution of graphene oxide.In addition, x-ray photoelectron power spectrum is adopted to characterize nano graphene oxide and graphene oxide raw material, the oxygen carbonatoms ratio of graphene oxide is 0.4830, the oxygen carbonatoms ratio of the nano graphene oxide after cutting is 0.4972, illustrates that cutting process does not cause remarkably influenced to the oxygen level of graphene oxide.These results suggest that, the degree of oxidation of ultrasonic cutting to graphene oxide has no significant effect.
Embodiment 2
0.5g graphene oxide raw material is added in 500mL water, at room temperature uses power 300W ultrasonic disperse 30 minutes, obtain finely dispersed suspension.Use power 600w supersound process suspension 9 hours, period controls solution temperature within the scope of 30 DEG C ~ 50 DEG C with water-bath.By the suspension after process be under the condition of 15000r/min centrifugal 30 minutes at centrifugation rate.By the centrifugal precipitation obtained 50 DEG C of vacuum-dryings 2 hours, obtain nano graphene oxide.Nano graphene oxide mean thickness is 1.90 ± 0.07nm, and mean diameter is 286 ± 29nm, and degree of oxidation is no significant difference compared with raw material.
Embodiment 3
0.1g graphene oxide raw material is added in 500mL water, at room temperature uses power 300W ultrasonic disperse 30 minutes, obtain finely dispersed suspension.Use power 700w supersound process suspension 5 hours, period controls solution temperature within the scope of 30 DEG C ~ 50 DEG C with water-bath.By the suspension after process be under the condition of 15000r/min centrifugal 30 minutes at centrifugation rate.The centrifugal precipitation obtained 50 DEG C is revolved steaming 4 hours, obtains nano graphene oxide.Nano graphene oxide mean thickness is 1.98 ± 0.12nm, and mean diameter is 439 ± 83nm, and degree of oxidation is no significant difference compared with raw material.
Embodiment 4
Add in 500mL water by 0.1g graphene oxide raw material, use power 800w supersound process 3 hours, period controls solution temperature within the scope of 30 DEG C ~ 50 DEG C with water-bath.By the suspension after process be under the condition of 10000r/min centrifugal 60 minutes at centrifugation rate.The centrifugal precipitation obtained 50 DEG C is revolved steaming 4 hours, obtains nano graphene oxide.Nano graphene oxide mean thickness is 2.08 ± 0.12nm, and mean diameter is 592 ± 156nm, and degree of oxidation is no significant difference compared with raw material.
Embodiment 5
Add in 500mL water by 0.1g graphene oxide raw material, use power 900w supersound process 1 hour, period controls solution temperature within the scope of 30 DEG C ~ 50 DEG C with water-bath.By the suspension after process be under the condition of 10000r/min centrifugal 60 minutes at centrifugation rate.The centrifugal precipitation obtained 50 DEG C is revolved steaming 4 hours, obtains nano graphene oxide.Nano graphene oxide mean thickness is 2.06 ± 0.07nm, and mean diameter is 921 ± 242nm, and degree of oxidation is no significant difference compared with raw material.
The present invention utilizes supersound process graphene oxide dispersion, thus the size of regulation and control graphene oxide, graphene oxide sheet diameter is cut to 300nm from 2500nm, and there is not considerable change in the degree of oxidation of graphene oxide.The present invention does not need to add chemical substance, low for equipment requirements, is the graphene oxide method of cutting out of a kind of efficient stable, simple to operate, mild condition, environmental protection.The operational hazards that instant invention overcomes traditional acidifying cutting and the existence of hydro-thermal method of cutting out is large, and environmental pollution is serious, and corrosive equipment, cost drops into high deficiency.Stannic oxide/graphene nano sheet prepared by the present invention has very wide application prospect in fields such as functional composite material, coating, ink, biological medicines.
Spoken of in this manual " embodiment ", " another embodiment ", " embodiment " etc., refer to the specific features, structure or the feature that describe in conjunction with this embodiment and be included at least one embodiment of the application's generality description.Multiple place occurs that statement of the same race is not necessarily refer to same embodiment in the description.Furthermore, when describing specific features, structure or a feature in conjunction with any one embodiment, what advocate is also fall within the scope of the invention to realize this feature, structure or feature in conjunction with other embodiments.
Although with reference to the multiple explanatory embodiment of inventing, invention has been described here, but, should be appreciated that, those skilled in the art can design a lot of other amendment and embodiment, these amendments and embodiment will drop within spirit disclosed in the present application and spirit.More particularly, in the scope of the open claim of the application, multiple modification and improvement can be carried out to the building block of subject combination layout and/or layout.Except the modification of carrying out building block and/or layout is with except improvement, to those skilled in the art, other purposes also will be obvious.
Claims (8)
1. a method for ultrasonic cutting graphene oxide, is characterized in that: described method comprises the following steps:
Step one: be added to the water by graphene oxide, obtains graphene oxide suspension;
Step 2: by the ultrasonic device process of graphene oxide suspension in step one, controls described graphene oxide suspension temperature within the scope of 30 DEG C ~ 50 DEG C;
Step 3: graphene oxide suspension in step 2 is carried out centrifugal treating, obtains graphene oxide precipitation;
Step 4: by dry for the precipitation of graphene oxide described in step 3, obtain nano graphene oxide sheet.
2. the method for ultrasonic cutting graphene oxide according to claim 1, it is characterized in that the graphene oxide in described step one is obtained by Brodie method, Staudenmaier method or Hummers method, described graphene oxide lamella diameter is 1000 ~ 5000nm.
3. the method for ultrasonic cutting graphene oxide according to claim 1, it is characterized in that in described step 2, ultrasonic power is 300w ~ 900w, ultrasonic time is 1h ~ 10h.
4. the method for ultrasonic cutting graphene oxide according to claim 1, is characterized in that in described step 2, graphene oxide suspension temperature adopts water-bath to control.
5. the method for ultrasonic cutting graphene oxide according to claim 1, it is characterized in that in described step 3, centrifugation rate is 10000r/min ~ 15000r/min, centrifugation time is 0.5h ~ 2h.
6. the method for ultrasonic cutting graphene oxide according to claim 1, to it is characterized in that in described step 4 that drying mode comprises and adopt vacuum drying oven dry or adopt and revolve that to steam instrument dry, drying temperature is 50 DEG C, and time of drying is 2 hours.
7. the method for ultrasonic cutting graphene oxide according to claim 1, is characterized in that the lamella diameter of described nano graphene oxide sheet is 220 ~ 370nm.
8. the method for the ultrasonic cutting graphene oxide according to claim 1 or 7, is characterized in that the degree of oxidation of described nano graphene oxide sheet is consistent with the degree of oxidation of described graphene oxide.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107128907A (en) * | 2017-05-04 | 2017-09-05 | 上海理工大学 | A kind of size classification method of improved graphene oxide and graphene |
| CN110683536A (en) * | 2019-06-20 | 2020-01-14 | 宁波锋成先进能源材料研究院 | Preparation method of graphene-based amphiphilic nano material |
| CN115721723A (en) * | 2022-09-13 | 2023-03-03 | 苏州大学附属第二医院 | Preparation method and application of fluorescent graphene oxide nano-membrane |
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| CN102701189A (en) * | 2012-05-11 | 2012-10-03 | 北京工业大学 | Method for nano-dispersing graphene oxide |
| CN103183334A (en) * | 2013-03-11 | 2013-07-03 | 上海理工大学 | Preparation method of size controllable grapheme |
| CN104803376A (en) * | 2015-03-27 | 2015-07-29 | 天津工业大学 | Efficient preparation process of graphene oxide nanosheets |
| CN104843695A (en) * | 2015-05-26 | 2015-08-19 | 山东大学 | Method for preparing two-dimensional nanosheet material through all-directional ultrasonic agitation process |
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- 2015-12-03 CN CN201510881904.4A patent/CN105293481A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701189A (en) * | 2012-05-11 | 2012-10-03 | 北京工业大学 | Method for nano-dispersing graphene oxide |
| CN103183334A (en) * | 2013-03-11 | 2013-07-03 | 上海理工大学 | Preparation method of size controllable grapheme |
| CN104803376A (en) * | 2015-03-27 | 2015-07-29 | 天津工业大学 | Efficient preparation process of graphene oxide nanosheets |
| CN104843695A (en) * | 2015-05-26 | 2015-08-19 | 山东大学 | Method for preparing two-dimensional nanosheet material through all-directional ultrasonic agitation process |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107128907A (en) * | 2017-05-04 | 2017-09-05 | 上海理工大学 | A kind of size classification method of improved graphene oxide and graphene |
| CN110683536A (en) * | 2019-06-20 | 2020-01-14 | 宁波锋成先进能源材料研究院 | Preparation method of graphene-based amphiphilic nano material |
| CN115721723A (en) * | 2022-09-13 | 2023-03-03 | 苏州大学附属第二医院 | Preparation method and application of fluorescent graphene oxide nano-membrane |
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