CN206858176U - A kind of liquid phase peel-off device for preparing two-dimension nano materials - Google Patents
A kind of liquid phase peel-off device for preparing two-dimension nano materials Download PDFInfo
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- CN206858176U CN206858176U CN201720705067.4U CN201720705067U CN206858176U CN 206858176 U CN206858176 U CN 206858176U CN 201720705067 U CN201720705067 U CN 201720705067U CN 206858176 U CN206858176 U CN 206858176U
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Abstract
The utility model provides a kind of liquid phase peel-off device for preparing two-dimension nano materials, including solvent tank, there is the cutter head and ultrasonic probe that emulsify dissection, the cutter head and ultrasonic probe are respectively positioned in solvent tank, cutter head is located at the height of solvent pot bottom 1/4~1/2, and ultrasonic probe is located at the height of solvent pot bottom 1/4~3/4.The utility model proposes device; mechanical stripping and ultrasound stripping is compound; can efficiently, cleaning peels off the layered solid powder in liquid phase into two-dimensional nano-film; such as graphene, molybdenum disulfide, black phosphorus nano flake; avoid using the harsh process conditions such as strong acid and strong base and HTHP; cost is relatively low, yield is higher, graphene or class graphene two-dimension nano materials suitable for prepare with scale high quality.
Description
Technical field
The invention belongs to field of energy source materials, and in particular to a kind of preparation facilities of two-dimension nano materials.
Background technology
Two-dimensional material refer to electronics only can on the non-nanosize (1-100nm) of two dimensions free movement material,
Such as nano thin-film, superlattices, SQW.Wherein graphene is two-dimensional material of greatest concern.From Univ Manchester UK
People have triggered to graphene and two dimension since the method synthesizing graphite alkene peeled off by micromechanics in 2004 in Geim seminar
The research boom of material, class graphene two-dimension nano materials, such as molybdenum disulfide nano thin slice, black phosphorus nano flake, because of its tool
There are good catalytic hydrogen evolution activity and storage lithium performance, there is potential application value in catalysis and energy storage field, also
Receive significant attention.
Graphene or class grapheme two-dimension material can be prepared by a variety of methods, can be largely classified into Physical and change
Method, wherein Physical can be divided into the methods of micromechanics is peeled off, liquid/vapor is directly peeled off, and chemical method can be divided into chemistry
The methods of vapour deposition (CVD), oxidation-reduction method.CVD method is to be deposited on solid film base by gas phase reaction under high temperature
The method of graphene on bottom, this method can prepare the graphene of high quality, large area, but higher cost, complicated technique
And harsh process regulation conditionality its development.Presently the most conventional oxide-reduction method, its general principle
It is that graphite is handled by strong protonic acid, forms compound between graphite layers, then adds strong oxidizer and it is aoxidized, form oxygen
Graphite alkene, redox graphene can be obtained by further reducing, but the method has used to changing in process of production
Construction equipment has severe corrosive, the strong acid and strong oxidizer of strong oxidizing property, has larger harm to environment, and form the electricity of graphene
By serious destruction, electrical conductivity has obvious reduction for minor structure and crystal perfection, limits it in the energy, electronic applications
In application and industrialized development.The method of liquid phase mechanical stripping can prepare the graphene and class graphene two of high quality
Dimension nano material, but typically peeled off by single mechanical stripping or ultrasonication, it is less efficient, and yield also compares
It is low.
The content of the invention
For weak point existing for this area, the purpose of the present invention is to propose to a kind of liquid phase for preparing two-dimension nano materials
Peel-off device, is by mechanically pulling off and compound action that ultrasound is peeled off, and safe efficient, stable will be scattered in liquid solution
In layered solid powder peel off into two-dimension nano materials, and prepared two-dimensional material have complete crystal structure, thickness of thin,
The advantages that adjustable controllable, specific surface area is big, yield is high.
The technical scheme for realizing the object of the invention is：
A kind of liquid phase peel-off device for preparing two-dimension nano materials, including solvent tank, the cutter head with emulsification dissection
And ultrasonic probe, the cutter head and ultrasonic probe are respectively positioned in solvent tank, cutter head is located at high apart from solvent pot bottom 1/4~1/2
At degree, probe is located at the height of solvent pot bottom 1/4~3/4.
In order to ensure cutter head and the equal normal work of probe, horizontal direction distance is in more than 5cm between cutter head and probe.
The utility model proposes device, by mechanical stripping and ultrasound peel off it is compound, can efficiently, clean by liquid phase
Layered solid powder peel off into two-dimensional nano-film, such as graphene, molybdenum disulfide, black phosphorus nano flake, avoid using strong
The harsh process conditions such as sour highly basic and HTHP, cost is relatively low, yield is higher, suitable for prepare with scale high quality
Graphene or class graphene two-dimension nano materials.
Wherein, the solvent tank is stainless steel, and the tank body of solvent tank is provided with chuck, and the chuck is connected with cooling
Water lines.
Further, the cutter head includes coaxial stator and rotor, a diameter of 8~12mm of stator, the diameter of rotor
For 12~16mm, radial direction spacing is 0.2~0.3mm between stator and rotor.
Preferably, the cutter head is connected with buncher, the distance between cutter head and ultrasonic probe in vertical direction be 1~
7cm, and ultrasonic probe is located at the top of cutter head.
Wherein, the ultrasonic probe is titanium alloy material, and ultrasonic probe is connected with supersonic generator.
The beneficial effects of the utility model are：
Present invention, avoiding be used alone emulsification cutting or ultrasonic device caused by charge stripping efficiency it is relatively low the problem of, energy
It is enough cleaned in the case of without using strong acid and severe corrosive chemical reagent, efficiently to separate thickness of thin, crystal structure complete
Whole, specific surface area is big and the adjustable controllable graphene of area and class graphene two-dimension nano materials.The present apparatus combines machine
The advantages of tool is peeled off and ultrasound is peeled off, can be by mechanically pulling off and the compound action of ultrasound is high by layered solid powder
Effect, the quick two-dimension nano materials peeled off into high quality, and there is no the discharge of dust, waste liquid, waste gas in stripping process.
Specifically,
1. the utility model is successfully compounded with mechanical shearing and ultrasonic release effect, stratiform powder body material is greatly improved
Charge stripping efficiency.
2. the present apparatus efficient under liquid-phase condition, cleaning can be peeled off layered solid material into two-dimension nano materials.
3. the two-dimension nano materials thickness of thin separated using the present apparatus, it is controllable that area is adjustable, and it is excellent that crystal structure is complete etc.
Point.
4. the utility model structure has the advantages that simple, cost is relatively low, energy consumption is small, commercial application can be carried out.
Brief description of the drawings
Fig. 1 is the liquid phase peel-off device structural representation of the utility model embodiment 1.
Fig. 2 is the liquid phase peel-off device structural representation of the utility model embodiment 2.
In figure, 1 is solvent tank, and 2 be cutter head, and 201 be buncher, and 202 be rotor, and 203 be stator, and 3 be ultrasonic probe,
301 be supersonic generator.
Embodiment
Detailed description below is used to illustrate the present invention, but should not be construed as limiting the invention.
In embodiment, unless otherwise instructed, technological means used is this area conventional technology.
Embodiment 1：
Referring to Fig. 1, a kind of liquid phase peel-off device for preparing two-dimension nano materials, including solvent tank 1, have emulsification cutting make
Cutter head 2 and ultrasonic probe 3, the height of solvent tank 1 is 20cm, and horizontal direction distance is about 5cm between cutter head and probe；Its
A diameter of 8mm of middle cutter head stator, a diameter of 12mm of rotor, the radial direction spacing between stator 203 and rotor 202 is about
0.2mm, distance of the cutter head apart from solvent tank bottom are about 5cm.Stator and rotor coaxial are set, its axis connection in buncher 201,
Buncher 201 is fixed on the top of solvent tank, and the rotating speed of buncher control rotor is adjustable between 1-18000 revs/min.Together
When by with ultrasonication titanium alloy probe be inserted into tank body, a diameter of about 6mm of ultrasonic probe 302, wherein bottom of popping one's head in
Portion is about 7cm apart from the distance of tank base, and ultrasonic probe 302 is connected to ultrasonic wave hair of the ultrasonic power between 1-1000W
Raw device 301.
The chuck of tank body is passed through cooling water, in time removes the heat of generation, the temperature of stripping solvent is remained stable.
Using the device of the present embodiment, the graphene nano materials process for preparing two dimension is：Added into solvent tank body molten
Agent about 1L, natural graphite powder about 100g, after stirring, mechanical shearing and ultrasonic peel-off device unit are opened simultaneously, its
For the rotating speed of middle mechanical shearing at 12000 revs/min, the power of ultrasonic stripping unit maintains 600W, and the temperature for peeling off solvent maintains
At 20 DEG C, by the working process of about 6 hours, high-quality graphene of the thickness in 1-10nm, and graphite can be successfully prepared
Alkene crystal structure is complete, and electrical conductivity is high.
Embodiment 2：
Such as Fig. 2, a kind of liquid phase peel-off device for preparing two-dimension nano materials, including solvent tank 1, there is emulsification dissection
Cutter head 2 and ultrasonic probe 3, the height of solvent tank 1 is 20cm, and horizontal direction distance is about 6cm between cutter head and probe.
To it be put into the cutter head that mechanical shearing acts in the stainless steel solvent tank with chuck, wherein cutter head stator
A diameter of 12mm, a diameter of 16mm of rotor, the radial distance between stator and rotor is about 0.3mm, and cutter head is apart from solvent tank
The distance at bottom is about 8cm, and buncher is located at below solvent tank, while the titanium alloy probe with ultrasonication is inserted into tank
In body, a diameter of 30mm of probe, wherein the distance of probe distance from bottom tank base is about 12cm, ultrasonic power is in 1-
Between 2000W, the chuck of tank body is passed through cooling water, in time removes the heat of generation, the temperature of stripping solvent is remained stable.
Solvent about 3L, molybdenum disulfide powder about 500g are added into solvent tank body, after stirring, by mechanical shearing and
Ultrasonic peel-off device unit is opened simultaneously, and wherein the rotating speed of mechanical shearing at 14000 revs/min, tie up by the power of ultrasonic stripping unit
Hold in 1400W, the temperature for peeling off solvent maintains 18 DEG C, is handled by the Continuous machings of about 8 hours, can successfully prepare thickness
The molybdenum disulfide two-dimension nano materials in 1-10nm are spent, and crystal structure is complete.
Embodiment 3：
In the present embodiment, a diameter of 12mm of cutter head stator, a diameter of 16mm of rotor, the radial direction between stator and rotor
Distance is about 0.2mm, and distance of the cutter head apart from solvent tank bottom is about 8cm, and the rotating speed of rotor is adjustable between 1-18000 revs/min
It is controllable.Titanium alloy probe with ultrasonication is inserted into tank body, a diameter of about 40mm of probe, wherein distance from bottom of popping one's head in
The distance of tank base is about 15cm, and ultrasonic power adjustable is controllable, and ultrasonic power is between 1-2000W.Other are set with real
Apply example 1.
Solvent about 5L, expanded graphite powder about 800g are added into solvent tank body, after stirring, by mechanical shearing and is surpassed
Sound peel-off device unit is opened simultaneously, and wherein at 13000 revs/min, the power of ultrasonic stripping unit maintains the rotating speed of mechanical shearing
In 1800W, the temperature for peeling off solvent maintains 18-22 DEG C, handles, can successfully prepare by the Continuous machings of about 12 hours
Thickness is in 1-8nm graphene, and crystal structure is complete, electrical conductivity is high.
Embodiment above is only that the embodiment of the present invention is described, and not the scope of the present invention is entered
Row limits, and those skilled in the art can also do numerous modifications and variations, be set not departing from the present invention on the basis of existing technology
On the premise of meter spirit, all variations and modifications that this area ordinary skill technical staff makes to technical scheme,
It all should fall into the protection domain of claims of the present invention determination.
Claims (5)
1. a kind of liquid phase peel-off device for preparing two-dimension nano materials, it is characterised in that including solvent tank, there is emulsification cutting to make
Cutter head and ultrasonic probe, the cutter head and ultrasonic probe are respectively positioned in solvent tank, and cutter head is located at apart from solvent pot bottom 1/4
At~1/2 height, ultrasonic probe is located at the height of solvent pot bottom 1/4~3/4.
2. liquid phase peel-off device according to claim 1, it is characterised in that the solvent tank is stainless steel, solvent
The tank body of tank is provided with chuck, and the chuck is connected with cooling water pipeline.
3. liquid phase peel-off device according to claim 1, it is characterised in that the cutter head includes coaxial stator and turned
Son, a diameter of 8~12mm of stator, a diameter of 12~16mm of rotor, between stator and rotor radial direction spacing be 0.2~
0.3mm。
4. the liquid phase peel-off device according to any one of claims 1 to 3, it is characterised in that the cutter head is connected with speed governing
Motor, the distance between cutter head and ultrasonic probe in vertical direction is 1~7cm, and ultrasonic probe is located at the top of cutter head.
5. the liquid phase peel-off device according to any one of claims 1 to 3, it is characterised in that the ultrasonic probe closes for titanium
Golden material, ultrasonic probe are connected with supersonic generator.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201720705067.4U CN206858176U (en) | 2017-06-16 | 2017-06-16 | A kind of liquid phase peel-off device for preparing two-dimension nano materials |
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| CN201720705067.4U CN206858176U (en) | 2017-06-16 | 2017-06-16 | A kind of liquid phase peel-off device for preparing two-dimension nano materials |
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| CN206858176U true CN206858176U (en) | 2018-01-09 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113148998A (en) * | 2021-06-04 | 2021-07-23 | 辛集市旭远新材料科技有限公司 | Graphene material production equipment and production method thereof |
-
2017
- 2017-06-16 CN CN201720705067.4U patent/CN206858176U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113148998A (en) * | 2021-06-04 | 2021-07-23 | 辛集市旭远新材料科技有限公司 | Graphene material production equipment and production method thereof |
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| GR01 | Patent grant | ||
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Effective date of registration: 20180523 Address after: 100024 Chaoyang District, Beijing, Chaoyang North Road, 1 D-2-8, Hong Chong International Cultural Innovation Park Patentee after: Beijing huakexun to graphene New Technology Research Institute Co. Ltd. Address before: 100035 No. 235 block A, 28 new street, new street, Xicheng District, Beijing. Co-patentee before: Beihang University Patentee before: Beijing huakexun to graphene New Technology Research Institute Co. Ltd. |
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Effective date of registration: 20180822 Address after: 214100 Dongsheng Road, anzhen Street City Industrial Park, Xishan District, Wuxi, Jiangsu, China Patentee after: YADEA TECHNIC GROUP CO.,LTD Address before: 100024 Chaoyang District, Beijing, Chaoyang North Road, 1 D-2-8, Hong Chong International Cultural Innovation Park Patentee before: Beijing huakexun to graphene New Technology Research Institute Co. Ltd. |
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Effective date of registration: 20201028 Address after: Room 8, unit 1, building 39, Luozhuang street, Muye District, Xinxiang City, Henan Province Patentee after: Li Ximei Address before: 214100 Dongsheng Road, anzhen Street City Industrial Park, Xishan District, Wuxi, Jiangsu, China Patentee before: YADEA SCIENCE & TECHNOLOGY GROUP Co.,Ltd. |
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Effective date of registration: 20220126 Address after: 100020 d-2-8 (1-3 floors), Beijing Hongzhuang international cultural bonded Innovation Park, No.1, baijialou, Chaoyang North Road, Chaoyang District, Beijing Patentee after: BEIJING HUAKE XUNNENG GRAPHENE NEW TECHNOLOGY RESEARCH INSTITUTE CO.,LTD. Address before: 453002 No.8, unit 1, building 39, Luozhuang street, Muye District, Xinxiang City, Henan Province Patentee before: Li Ximei |