CN105948024B - The preparation method of macroscopical aggregation of micro Nano material - Google Patents
The preparation method of macroscopical aggregation of micro Nano material Download PDFInfo
- Publication number
- CN105948024B CN105948024B CN201610275584.2A CN201610275584A CN105948024B CN 105948024 B CN105948024 B CN 105948024B CN 201610275584 A CN201610275584 A CN 201610275584A CN 105948024 B CN105948024 B CN 105948024B
- Authority
- CN
- China
- Prior art keywords
- micro
- nano
- gradually reducing
- reducing pipeline
- nano material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Landscapes
- Carbon And Carbon Compounds (AREA)
- Colloid Chemistry (AREA)
Abstract
The present invention relates to a kind of preparation method of macroscopical aggregation of micro Nano material, it comprises the following steps：A gradually reducing pipeline is provided, the internal diameter of the gradually reducing pipeline tapers into along the bearing of trend of the gradually reducing pipeline, and one end that the internal diameter of the gradually reducing pipeline is larger is defined as entrance, and the less one end of internal diameter is defined as exporting, and has multiple perforates on the tube wall of the gradually reducing pipeline；A micro-nano unit dispersion liquid is provided, the dispersion liquid includes solvent and the micro-nano unit being dispersed in the solvent；And the micro-nano unit dispersion liquid is flowed from the entrance of the gradually reducing pipeline to export direction, and make to remove solvent while the micro-nano unit dispersion liquid shear flow.This method is adapted to produce in batches, compared with other technologies from bottom to top, is a kind of high flux, inexpensive technology, is adapted to large-scale industrial production.
Description
Technical field
The invention belongs to nanometer technique field, more particularly to a kind of preparation method of macroscopical aggregation of micro Nano material
And preparation facilities.
Background technology
Basic construction unit is typically micro-meter scale in macroscopical aggregation of the micro Nano materials such as graphene, CNT
Sp2Carbon structure.This microcosmic texture characteristic determines that assembled material need to be by micro nano structure interphase interaction in stress
Transmit load.Research shows that the ordered arrangement of micro nano structure can help the transmission of the load of interlayer.But current take out
The process technologies such as filter, spinning can not obtain the high-sequential of micro Nano material, fine and close macroscopical aggregation, the microcosmic knot of its assembly
Structure is loose, structures shape performance, so the material property and ideal situation gap that obtain are larger.
In the Nature, spider spue silk there is extremely strong toughness and intensity, be known most outstanding material it
One, its microscopic units high-sequential formed arrangement.Spider makes microcosmic group in spinning moment, liquid flowing generation shear rate field
Into cell height ordered arrangement, therefore there is excellent performance.Based on this, the present invention proposes flowing, the steaming that a kind of biology inspires
Send out package technique.Make graphene, CNT by controlling evaporation, pressure difference and line size to produce controllable shear flow velocity field
Macroscopical aggregation that microstructure meets above-mentioned requirements is assembled into Deng substantially micro-nano unit.
The content of the invention
The present invention provides a kind of preparation method of macroscopical aggregation of micro Nano material.
A kind of preparation method of macroscopical aggregation of micro Nano material, it comprises the following steps：One gradually reducing pipeline is provided, should
The internal diameter of gradually reducing pipeline tapers into along the bearing of trend of the gradually reducing pipeline, and one end that the internal diameter of the gradually reducing pipeline is larger defines
For entrance, the less one end of internal diameter is defined as exporting, and has multiple perforates on the tube wall of the gradually reducing pipeline；It is micro-nano to provide one
Unit dispersion liquid, the dispersion liquid include solvent and the micro-nano unit being dispersed in the solvent；And make this micro-nano
Unit dispersion liquid flows from the entrance of the gradually reducing pipeline to export direction, and makes the micro-nano unit dispersion liquid shear flow
Remove solvent simultaneously.
Such as preparation method of macroscopical aggregation of above-mentioned micro Nano material, wherein, the micro-nano unit is one-dimensional micro-nano
One or more in rice material and two-dimentional micro Nano material.
Such as preparation method of macroscopical aggregation of above-mentioned micro Nano material, wherein, the one-dimensional micro-nanometer material is received for carbon
Mitron；The two-dimentional micro Nano material is graphene.
Such as preparation method of macroscopical aggregation of above-mentioned micro Nano material, wherein, the full-size of the micro Nano material
More than size of the perforate along the gradually reducing pipeline bearing of trend.
Such as preparation method of macroscopical aggregation of above-mentioned micro Nano material, wherein, the solvent is in water and organic solvent
One or more；And the gradually reducing pipeline is the non-slip flow body pipeline relative to the solvent.
Such as preparation method of macroscopical aggregation of above-mentioned micro Nano material, wherein, the micro-nano unit dispersion liquid is in institute
State and be full of whole gradually reducing pipeline in radial direction during being flowed in gradually reducing pipeline；The micro-nano unit is by shear flow and edge
After flow direction ordered arrangement, then make to remove solvent while the micro-nano unit dispersion liquid shear flow.
Such as preparation method of macroscopical aggregation of above-mentioned micro Nano material, wherein, the method for removing solvent is to pass through
Heating makes solvent evaporated from the multiple perforate.
Such as preparation method of macroscopical aggregation of above-mentioned micro Nano material, wherein, the method for removing solvent is molten to make
Agent is permeable by the multiple perforate.
Such as preparation method of macroscopical aggregation of above-mentioned micro Nano material, wherein, in the micro-nano unit dispersion liquid
Micro-nano unit forms macroscopical aggregation of micro Nano material after removal of solvents；Further, by the grand of the micro Nano material
Aggregation is seen to release to form a micro Nano material fiber from outlet；While the macroscopic view for the micro Nano material for exporting side is assembled
Body is extracted out, while from the new micro-nano unit dispersion liquid of inlet side injection, continuously prepares micro Nano material fiber.
Such as preparation method of macroscopical aggregation of above-mentioned micro Nano material, wherein, when in the micro-nano unit dispersion liquid
After micro-nano unit concentration reaches certain value, the micro-nano unit dispersion liquid freezes to form one prefabricated by refrigerating plant
Body；Then after the precast body is taken out, the solvent of residual is removed by distilling, obtains macroscopical aggregation of micro Nano material.
The preparation method of macroscopical aggregation provided by the invention, there is advantages below：One, by controlling tapered fluid pipe
The pressure difference in road can be with the shear rate size in control pipeline, so as to control micro-nano unit arrangement order, therefore, Ke Yitong
Flow field in the external condition such as overpressure difference and line size control fluid line, and then manipulate micro Nano material macroscopic view assembly
Microstructure order and density.Secondly, micro-nano unit after shear flow is orderly, removed while shear flow molten
Agent simultaneously keeps shearing force constant, and the cooperative effect of flowing and removal solvent makes the order of micro-nano unit not be destroyed, so as to
It ensure that the order of the micro-nano unit in macroscopical aggregation of micro Nano material.Thirdly, fluid media (medium) be readily available, pipeline
Process technology is ripe, is adapted to batch production, is a kind of high flux compared with other technologies from bottom to top, inexpensive technology,
It is adapted to large-scale industrial production.
Brief description of the drawings
Fig. 1 is the structural representation of the preparation facilities of the macroscopical aggregation for the micro Nano material that the embodiment of the present invention 1 provides.
Fig. 2 is the structural representation of the preparation facilities of the macroscopical aggregation for the micro Nano material that the embodiment of the present invention 2 provides.
Fig. 3 is the structural representation of the preparation facilities of the macroscopical aggregation for the micro Nano material that the embodiment of the present invention 3 provides.
Fig. 4 is the Flow Field Distribution schematic diagram in the gradually reducing pipeline of the embodiment of the present invention.
Fig. 5 is the order and Peclet number (Peclet of the micro-nano unit in the gradually reducing pipeline of the embodiment of the present invention
Number), the graph of a relation of shear rate.
Fig. 6 is the unordered micro nanometer fiber unit being scattered in solution of the embodiment of the present invention through the shearing of piping flow field, steaming
It is changed into the orderly, numerical simulation result of compact texture after hair.
Fig. 7 is the micro-nano unit dispersion liquid institute in the gradually reducing pipeline of embodiment of the present invention when not considering the evaporation of solvent
Distribution of the pressure difference being subject to along duct length x and the relation with the pipeline gradient β of the gradually reducing pipeline.
Fig. 8 is the micro-nano unit dispersion liquid institute in the gradually reducing pipeline of embodiment of the present invention when not considering the evaporation of solvent
Distribution of the shear rate being subject to along duct length x and with the shape of the gradually reducing pipeline, size, gradient β and entrance
Export pressure differential deltap p relation.
Fig. 9 is when considering the evaporation of solvent, suffered by the micro-nano unit dispersion liquid in the gradually reducing pipeline of the embodiment of the present invention
Distribution of the shear rate arrived along duct length x and the relation with the gradient β of the gradually reducing pipeline.
Main element symbol description
| The preparation facilities of macroscopical aggregation of micro Nano material | 10, 10A, 10B |
| Container | 12 |
| Device for exerting | 14 |
| Gradually reducing pipeline | 16 |
| Entrance | 160 |
| Outlet | 162 |
| Perforate | 164 |
| Valve | 18 |
| Heater | 17 |
| Refrigerating plant | 19 |
| Micro-nano unit dispersion liquid | 20 |
| Solvent | 22 |
| Micro-nano unit | 24 |
| Macroscopical aggregation of micro Nano material | 26 |
| Precast body | 28 |
Following embodiment will combine above-mentioned accompanying drawing and further illustrate the present invention.
Embodiment
Illustrate macroscopical aggregation of micro Nano material provided by the invention below with reference to above-mentioned accompanying drawing and different embodiments
Preparation method and preparation facilities.
Referring to Fig. 1, the preparation facilities 10 of macroscopical aggregation of micro Nano material provided in an embodiment of the present invention includes：One holds
Device 12, a device for exerting 14 and a gradually reducing pipeline 16.
The container 12 is used to hold micro-nano unit dispersion liquid 20.The micro-nano unit dispersion liquid 20 includes solvent 22
And it is dispersed in the micro-nano unit 24 in the solvent 22.The device for exerting 14 is connected with the container 12, for this
Micro-nano unit dispersion liquid 20 in container 12 applies pressure so that the micro-nano unit dispersion liquid 20 can along it is described gradually
Pipe 16 flows.The gradually reducing pipeline 16 is connected with the container 12, for the micro-nano unit dispersion liquid to its internal flow
20 form a Shearing Flow, so that the micro-nano unit 24 in the micro-nano unit dispersion liquid 20 of the flowing is in the Shearing Flow
Along flow direction ordered arrangement under effect.Moreover, the gradually reducing pipeline 16 can also be in the micro-nano unit 24 along flowing
After the ordered arrangement of direction, keep the micro-nano unit dispersion liquid 20 to continue to flow, and sheared in the micro-nano unit dispersion liquid 20
The solvent 22 of the micro-nano unit dispersion liquid 20 is gradually removed while flowing, it is micro- so as to obtain one in the gradually reducing pipeline 16
Macroscopical aggregation 26 of nano material.
The shape of the container 12, size and structure are unlimited, can design as needed.The material of the container 12 can be with
There is the material of certain degree of hardness and intensity for metal, ceramics, glass, quartz or polymer etc..
The device for exerting 14 can apply pressure to be any to the micro-nano unit dispersion liquid 20 in the container 12
Device.The position that the device for exerting 14 is set is unlimited, can select as needed.
Bearing of trend of the internal diameter of the gradually reducing pipeline 16 along the gradually reducing pipeline 16 tapers into.The present invention is tapered by this
One end that the internal diameter of pipeline 16 is larger is defined as entrance 160, and the less one end of internal diameter is defined as outlet 162.Preferably, it is described gradually
The internal diameter of pipe 16 tapers into from entrance 160 to outlet 162.The entrance 160 of the gradually reducing pipeline 16 passes through a valve 18
Connected with the container 12.The entrance 160 and 162 sizes of outlet of the gradually reducing pipeline 16 are unlimited, can design as needed.It is described
The material of gradually reducing pipeline 16 can be the material that metal, ceramics, glass, quartz or polymer etc. have certain degree of hardness and intensity.
The shape of cross section of the gradually reducing pipeline 16 is unlimited, can be circle, ellipse, triangle, square, rectangle, Yi Jiqi
His N sides shape, N≤5.The length of the gradually reducing pipeline 16 is unlimited, can design as needed.It is appreciated that the gradually reducing pipeline
16 length need to ensure that the micro-nano unit dispersion liquid 20, along after the ordered arrangement of flow direction, is protected under Shearing Flow effect
Hold the micro-nano unit dispersion liquid 20 to continue to flow, and gradually removed while micro-nano 20 shear flow of unit dispersion liquid
The solvent 22 of the micro-nano unit dispersion liquid 20.Preferably, the gradually reducing pipeline 16 is without sliding relative to the solvent 22
Fluid line.The section of the gradually reducing pipeline 16 alongst can be two spaced straight lines or camber line.It is described
The time of the gradients affect flow evaporation of gradually reducing pipeline 16, this also influences final pattern.Gradient, which crosses conference, causes shearing not filled
Point, may not high-sequential.The gradient of the gradually reducing pipeline 16 is related to length and the diameter of gateway 160.It is described
It can also be Split type structure that gradually reducing pipeline 16, which can be structure as a whole,.Preferably, the gradually reducing pipeline 16 uses Split type structure, with
It is easy to subsequently take out the macroscopical aggregation 26 for the micro Nano material for being deposited on its inwall, and its inwall is cleaned.
Preferably, the multi-segment structure that the gradually reducing pipeline 16 can alongst be divided into, fit together during use.Further,
Each segment pipe can also be two valves or more valve structures, fit together during use.It is appreciated that the gradually reducing pipeline 16 also may be used
A part for other non-tapered pipelines is thought, as long as the purpose of the present invention can be realized in the part of the gradually reducing pipeline 16.
There are multiple perforates 164, for removing the micro-nano unit dispersion liquid 20 on the tube wall of the gradually reducing pipeline 16
Solvent 22.The shape of perforate 164 is unlimited, can be circle, ellipse, triangle, square, rectangle etc..The perforate
164 size and density can be according to the size selection of the micro-nano unit 24.Pass through the size and density of the perforate 164
The speed for the solvent 22 for removing the micro-nano unit dispersion liquid 20 can be controlled.Preferably, the perforate 164 is along the reducing pipe
The size of the bearing of trend in road 16 should be more than the full-size of the micro-nano unit 24, such as the length of one-dimensional micro-nanometer material
Degree, to prevent the micro-nano unit 24 from being spilt out with solvent 22 from the perforate 164.It is it is appreciated that a range of few
Perhaps micro-nano unit outflow can also receive.The multiple perforate 164 can be set along radially around the gradually reducing pipeline 16,
It can also be only arranged on one or more tube walls of the gradually reducing pipeline 16.It is appreciated that when the micro-nano unit disperses
Liquid 20, which enters after the gradually reducing pipeline 16, it is necessary to flow a period of time, can shear the micro-nano unit dispersion liquid 20
Along flow direction ordered arrangement under the effect of flow field.Therefore, the front section in the gradually reducing pipeline 16 close to entrance 160, no
Need to set perforate 164.That is, the multiple perforate 164 can axially/length direction be only arranged at it is described tapered
Hindfoot portion of the pipeline 16 close to outlet 162.
Referring to Fig. 2, the preparation facilities 10 of macroscopical aggregation of the micro Nano material can also include a heater 17,
For heating the micro-nano unit dispersion liquid 20 in the gradually reducing pipeline 16.The structure and set location of the heater 17 are not
Limit, can be designed as needed.
Referring to Fig. 3, the preparation facilities 10 of macroscopical aggregation of the micro Nano material can also include a refrigerating plant 19,
For freezing the micro-nano unit dispersion liquid 20 in the gradually reducing pipeline 16.The structure and set location of the refrigerating plant 19 are not
Limit, can be designed as needed.
The solvent 22 can be the one or more in water and organic solvent.The solvent 22 can also be the poly- of fusing
Compound or metal.The organic solvent is one or more kinds of in methanol, ethanol, acetone, dichloroethanes and chloroform.The micro-nano
Meter Dan Yuan 24 can be the one or more in one-dimensional micro-nanometer material and two-dimentional micro Nano material.The one-dimensional micro-nanometer material
Can be the one or more in micro-nano pipe, micro-nano rice noodles, micro-and nanorods and micro-nano band.The two-dimentional micro Nano material
For the one or more in micro-nano, micro-nano film and micro-nano layer.Can be with the micro-nano unit dispersion liquid 20
Further comprise dispersant or surfactant, so that the micro-nano unit 24 is dispersed, do not reunite.It is described micro-
Nano unit 24 can be dispersed in solvent 22 by ultrasound.
The preparation facilities 10 or 10A of macroscopical aggregation introduced below using micro Nano material provided by the invention prepare micro-
The method of macroscopical aggregation 26 of nano material, this method include：Make the micro-nano unit dispersion liquid 20 from the gradually reducing pipeline
16 entrance 160 flows to 162 directions of outlet；And make to remove solvent while micro-nano 20 shear flow of unit dispersion liquid
22.Preferably, the micro-nano unit 24 is by shear flow and along after the ordered arrangement of flow direction, then makes the micro-nano unit
Solvent 22 is removed while 20 shear flow of dispersion liquid.
In the above method, the micro-nano unit dispersion liquid 20 is in the gradually reducing pipeline 16 radially during flowing
Full of whole gradually reducing pipeline 16.Preferably, the gradually reducing pipeline 16 is the non-slip flow body pipeline relative to the solvent 22.By
In the fluid close to the tube wall of gradually reducing pipeline 16 easily by the shearing force of tube wall, and positioned at the center of gradually reducing pipeline 16
Fluid is not readily susceptible to the shearing force of tube wall, and the present invention is it is highly preferred that the solvent 22 has certain viscosity, so that institute
The fluid for stating everywhere in gradually reducing pipeline 16 can be by shearing force.The method for removing solvent 22 is makes solvent 22 pass through institute
It is permeable to state multiple perforates 164, or makes solvent 22 evaporated from the multiple perforate 164 by heating.The reducing pipe
Pressure difference is formed between the entrance 160 in road 16 and outlet 162.It is appreciated that the micro-nano list can be controlled by the pressure difference
The density of macroscopical aggregation 26 of the flow of first dispersion liquid 20 and the micro Nano material of acquisition.The micro Nano material of the acquisition
Macroscopical aggregation 26 can be taken out at the outlet 162 of the gradually reducing pipeline 16, or by the way that the gradually reducing pipeline 16 is opened
Take out.
The principle of the preparation method of macroscopical aggregation of micro Nano material provided by the invention introduced below.
After the entrance 160 of micro-nano unit dispersion liquid 20 from the gradually reducing pipeline 16 is passed through, the reducing pipe
The VELOCITY DISTRIBUTION of micro-nano unit dispersion liquid 20 in road 16 is as shown in Figure 4.Now, the gradient of speed is shear rate, described
The average shear rate γ of gradually reducing pipeline 16 can use below equation (1) to describe：
γ=Q/dw2 (1)
Wherein Q is the flow of the micro-nano unit dispersion liquid 20, d and w be respectively the gradually reducing pipeline 16 depth and
Width.As can be seen here, in the case of equal flow, the radial dimension of gradually reducing pipeline 16 is smaller, can obtain higher cut
Cutting speed rate.Wherein, the flow of the micro-nano unit dispersion liquid 20 is by the size of the gradually reducing pipeline 16 and the pressure difference control at both ends
System.And the pressure difference at the both ends of gradually reducing pipeline 16 is controlled by the device for exerting 14.Therefore, the flow field of the gradually reducing pipeline 16
Distribution can be regulated and controled by regulating and controlling size and the device for exerting 14 of the gradually reducing pipeline 16.
Shearing force and thermal agitation of the micro-nano unit 24 in fluid by Shearing Flow in the gradually reducing pipeline 16.Two
The intensity ratio of person can be weighed with Peclet number Pe, be expressed as formula (2)：
Pe = γ/D (2)
Wherein D is the rotational diffusion coefficient for the micro-nano unit 24 for weighing thermal agitation effect-size.Peclet number and shearing
Speed is linear relationship.The order of the micro-nano unit 24 in fluid in the gradually reducing pipeline 16 and the close phase of Peclet number
Close, under two-dimensional case, order O is represented with equation below (3)：
O = <2cos2θ −1> (3)
Wherein θ is the micro-nano unit 24 axially angle with flow velocity direction.When disorder distribution, O value is 0；
θ=0 when the limit is orderly, O value are 1.As shown in figure 5, in the case where not considering the micro-nano inertia effect of unit 24,
Shear rate is bigger, and Peclet number is bigger, and order is higher.Therefore, can be by controlling flow field shear rate to control pik
Columns, and then adjust the order of micro-nano 24 macroscopical assembly of unit.
After the micro-nano unit 24 is clipped orderly in the gradually reducing pipeline 16, flow of fluid is kept simultaneously to start
Except solvent 22, i.e. the solvent 22 discharges the gradually reducing pipeline 16 by perforate 164.Due to solvent in the gradually reducing pipeline 16
22 reduction, cause the reduction of flow, can keep flowing shear rate using gradually reducing pipeline, so as to keep the micro-nano in fluid
Meter Dan Yuan 24 order.Simultaneously as the reduction of solvent 22, the concentration increase of the micro-nano unit 24 in fluid, so as to obtain
Obtain macroscopical aggregation 26 of fine and close micro Nano material.It is the unordered micro-nano being scattered in solution of the embodiment of the present invention referring to Fig. 6
Rice fiber element is changed into orderly, compact texture numerical simulation result after the shearing of piping flow field, evaporation.
The shape of the gradually reducing pipeline 16, size, pressure, the relationship analysis of shear rate are as follows.Assuming that at entrance 160
Pressure is p1, the pressure exported at 162 is p2, the height of entrance 160 is h1, the height for exporting 162 is h2.So it is described gradually
The pressure difference of pipe 16 is Δ p=p1 – p2。
When not considering the evaporation of solvent 22, the shear rate in the gradually reducing pipeline 16 is distributed as：
(4)
Wherein, μ is the viscosity of the micro-nano unit dispersion liquid 20 in above formula (4).Fig. 7 is in the gradually reducing pipeline 16
Distribution of the pressure difference along duct length x suffered by micro-nano unit dispersion liquid 20 and the pipeline with the gradually reducing pipeline 16
Gradient β relation, wherein, 0≤x≤L, β=h2/h1.Fig. 8 is suffered by the micro-nano unit dispersion liquid 20 in the gradually reducing pipeline 16
Distribution of the shear rate arrived along duct length x and with the shape of the gradually reducing pipeline 16, size, gradient β and entrance
Pressure differential deltap p relation is exported, wherein, Fig. 85 examples of having passed the imperial examinations at the provincial level illustrate their relation.
When considering the evaporation of solvent 22, the shear rate distribution in the gradually reducing pipeline 16 is as shown in Figure 9.Such as Fig. 9 borders
Shown in dotted line, when no solvent 22 evaporates along gradually reducing pipeline 16, due to being gradually reducing pipeline, shear rate from entrance 160 to
Outlet 162 is continuously increased.As Fig. 9 borders are shown in solid, when solvent 22, which reaches outlet 162, all to evaporate, shear rate
Constantly reduce from entrance 160 to outlet 162, and it is 0 to export the shear rate at 162.Other situations all fall in dotted line and solid line
The region of envelope.Fig. 9 sets forth under three kinds of different gradient β, the contrast of the shear rate distribution in the gradually reducing pipeline 16.
It can be seen that pipeline gradient β is bigger, shear rate changes in distribution is also more violent.
It is appreciated that the micro-nano unit 24 that will can be distributed in order in the gradually reducing pipeline 16 using the method for the present invention
The solvent 22 at place all removes, and obtains macroscopical aggregation 26 of a micro Nano material.It is appreciated that solvent 22 obtains after all removing
To macroscopical aggregation 26 of micro Nano material be easily adsorbed on the inwall of gradually reducing pipeline 16, and be not easy and the reducing pipe
Road 16 separates.Using the method for the present invention the micro-nano unit 24 being distributed in order in the gradually reducing pipeline 16 can also be waited to reach one
Determine to take out to obtain a precast body after concentration value, reheat the precast body.The precast body easily divides with the gradually reducing pipeline 16
From.The order that the micro-nano unit 24 arranges can determine calculating, by way of measuring.What this was distributed in order
The concentration of micro-nano unit 24 can be by determining total steaming of the micro-nano concentration of unit dispersion liquid 20 and solvent 22 at entrance 160
Hair amount determines.
The preparation method of macroscopical aggregation of micro Nano material provided by the invention has advantages below：One, pass through control
The pressure difference of tapered fluid pipeline processed can be with the shear rate size in control pipeline, so as to control micro-nano unit arrangement orderly
Property, therefore, the flow field in fluid line can be controlled by external conditions such as pressure difference and line sizes, and then manipulate micro-nano material
Expect the microstructure order and density of macroscopical assembly.Secondly, micro-nano unit after shear flow is orderly, in shear flow
Solvent is removed while dynamic and keeps shearing force constant, the cooperative effect of flowing and removal solvent makes the order of micro-nano unit
It is not destroyed, ensures that the order of the micro-nano unit in macroscopical aggregation of micro Nano material.Thirdly, fluid media (medium)
It is readily available, pipeline processing technology maturation, is adapted to batch production, is a kind of high flux compared with other technologies from bottom to top,
The technology of low cost, it is adapted to large-scale industrial production.
It is below the specific embodiment of the present invention
Embodiment 1
Referring to Fig. 1, the preparation facilities 10 of macroscopical aggregation of the micro Nano material used for the embodiment of the present invention 1.This reality
Apply in example, the container 12 is rectangle steel vessel.The device for exerting 14 is a piston, by piston to the bottom of container 12
Motion, so as to apply pressure to the micro-nano unit dispersion liquid 20 in the container 12.In the present embodiment, the gradually reducing pipeline 16
It is circular quartz ampoule for cross section.The multiple perforate 164 is circle, and is set along radially around the gradually reducing pipeline 16
Put.The multiple perforate 164 is micron order size.The micro-nano unit dispersion liquid 20 is by dispersing graphene in shape in water
Into.
In the present embodiment, the method for preparing macroscopical aggregation 26 of micro Nano material is：First, by the micro-nano of graphene
Unit dispersion liquid 20 is placed in the container 12；Secondly, valve 18 is opened, and is made by the device for exerting 14 described micro-nano
Unit dispersion liquid 20 is from the entrance 160 of the gradually reducing pipeline 16 to the flowing of 162 directions of outlet；Then, the micro-nano unit 24
Along after the ordered arrangement of flow direction after shear flow, pass through while micro-nano 20 shear flow of unit dispersion liquid
Perforate 164 infiltration remove solvent 22, so as to obtain a graphene in order and dense arrangement micro Nano material macroscopical aggregation
26, and macroscopical aggregation 26 of the micro Nano material is deposited on the inwall of the gradually reducing pipeline 16；Finally, open described tapered
Pipeline 16 takes out macroscopical aggregation 26 of the micro Nano material.
Embodiment 2
Referring to Fig. 2, the preparation facilities 10A of macroscopical aggregation of the micro Nano material used for the embodiment of the present invention 2.This hair
The preparation facilities 10A of the macroscopical aggregation for the micro Nano material that bright embodiment 2 uses uses micro-nano with the embodiment of the present invention 1
The structure of the preparation facilities 10 of macroscopical aggregation of material is essentially identical, and it is distinguished as, the gradually reducing pipeline 16 for cross section
To be square, and the multiple perforate 164 only set with the top surface of the gradually reducing pipeline 16 on；Further, a heater 17 is set
It is placed in the outer surface of the gradually reducing pipeline 16.In the present embodiment, the heater 17 is resistive heater, and it is wrapped in described
The outer surface of gradually reducing pipeline 16.Be arranged at intervals between adjacent two circle of the resistance wire, and the multiple perforate 164 be arranged at it is adjacent
Two circles between.
In the present embodiment, the micro-nano unit dispersion liquid 20 is formed by the way that CNT is scattered in ethanol.It is described
The method for preparing macroscopical aggregation 26 of micro Nano material is：First, the micro-nano unit dispersion liquid 20 of CNT is placed in
In the container 12；Secondly, valve 18 is opened, and the micro-nano unit dispersion liquid 20 is made from institute by the device for exerting 14
The entrance 160 for stating gradually reducing pipeline 16 flows to 162 directions of outlet；Then, the edge after shear flow of micro-nano unit 24
After flow direction ordered arrangement, heating evaporation removes solvent 22 while micro-nano 20 shear flow of unit dispersion liquid,
So as to obtain a CNT in order and dense arrangement micro Nano material macroscopical aggregation 26.Further, in the present embodiment,
Macroscopical aggregation 26 of the micro Nano material is released to form a micro Nano material fiber from outlet 162 by a clip.
As long as it is appreciated that while the macroscopical aggregation 26 of micro Nano material for exporting 162 sides is extracted out, while from entrance 160 1
The new micro-nano unit dispersion liquid 20 of side injection, it is possible to continuously prepare micro Nano material fiber.
Embodiment 3
Referring to Fig. 3, the preparation facilities 10B of macroscopical aggregation of the micro Nano material used for the embodiment of the present invention 3.This hair
The preparation facilities 10B of the macroscopical aggregation for the micro Nano material that bright embodiment 3 uses uses micro-nano with the embodiment of the present invention 1
The structure of the preparation facilities 10 of macroscopical aggregation of material is essentially identical, and it is distinguished as, and the multiple perforate 164 is only set and institute
State one section of the centre of gradually reducing pipeline 16；Further, a refrigerating plant 19 is arranged at the gradually reducing pipeline 16 close to the one of outlet 162
Section.The gradually reducing pipeline 16 to should one section of refrigerating plant 19 there is no perforate 164.
In the present embodiment, the micro-nano unit dispersion liquid 20 to be formed by the way that CNT is dispersed in water.The system
The method of macroscopical aggregation 26 of standby micro Nano material is：First, the micro-nano unit dispersion liquid 20 of CNT is placed in institute
State in container 12；Secondly, valve 18 is opened, and the micro-nano unit dispersion liquid 20 is made from described by the device for exerting 14
The entrance 160 of gradually reducing pipeline 16 flows to 162 directions of outlet；Then, the micro-nano unit 24 after shear flow along
It is molten by the infiltration removal of perforate 164 while micro-nano 20 shear flow of unit dispersion liquid after the ordered arrangement of flow direction
Agent 22, so as to obtain the micro-nano unit dispersion liquid 20 of a CNT ordered arrangement；When in the micro-nano unit dispersion liquid 20
Carbon nanotube concentration reach certain value after, the micro-nano unit dispersion liquid 20 freezes to form one pre- by refrigerating plant 19
Body 28 processed, after then the precast body 28 is taken out, the solvent 22 of residual is removed by distilling, the macroscopic view for obtaining micro Nano material is gathered
Collective 26.
The various embodiments described above are that present invention is described further, and should not be construed as the scope of the present invention and are only limitted to
Embodiment is stated, it is all that the scope of protection of the invention is belonged to based on the technology that the above is realized.In addition, those skilled in the art
Other changes can also be done in spirit of the invention, these changes done according to present invention spirit, should all be included in the present invention
In claimed scope.
Claims (10)
1. a kind of preparation method of macroscopical aggregation of micro Nano material, it comprises the following steps：
A gradually reducing pipeline is provided, the internal diameter of the gradually reducing pipeline tapers into along the bearing of trend of the gradually reducing pipeline, the reducing pipe
One end that the internal diameter in road is larger is defined as entrance, and the less one end of internal diameter is defined as exporting, and has on the tube wall of the gradually reducing pipeline
There are multiple perforates, the multiple perforate is alongst only arranged at hindfoot portion of the gradually reducing pipeline close to outlet, and
In the gradually reducing pipeline perforate is not provided with close to the front section of entrance；
A micro-nano unit dispersion liquid is provided, the dispersion liquid includes solvent and the micro-nano list being dispersed in the solvent
Member；And
The micro-nano unit dispersion liquid is flowed from the entrance of the gradually reducing pipeline to export direction, disperse the micro-nano unit
Solvent is removed while liquid shear flow.
2. the preparation method of macroscopical aggregation of micro Nano material as claimed in claim 1, it is characterised in that described micro-nano
Unit is the one or more in one-dimensional micro-nanometer material and two-dimentional micro Nano material.
3. the preparation method of macroscopical aggregation of micro Nano material as claimed in claim 2, it is characterised in that described one-dimensional micro-
Nano material is CNT；The two-dimentional micro Nano material is graphene.
4. the preparation method of macroscopical aggregation of micro Nano material as claimed in claim 1, it is characterised in that described micro-nano
The full-size of material is more than size of the perforate along the gradually reducing pipeline bearing of trend.
5. the preparation method of macroscopical aggregation of micro Nano material as claimed in claim 1, it is characterised in that the solvent is
One or more in water and organic solvent；And the gradually reducing pipeline is the non-slip flow body pipeline relative to the solvent.
6. the preparation method of macroscopical aggregation of micro Nano material as claimed in claim 1, it is characterised in that described micro-nano
Unit dispersion liquid is radially being full of whole gradually reducing pipeline during being flowed in the gradually reducing pipeline；The micro-nano unit warp
Cross shear flow and along after the ordered arrangement of flow direction, then make to remove while the micro-nano unit dispersion liquid shear flow molten
Agent.
7. the preparation method of macroscopical aggregation of micro Nano material as claimed in claim 1, it is characterised in that the removal is molten
The method of agent is to make solvent evaporated from the multiple perforate by heating.
8. the preparation method of macroscopical aggregation of micro Nano material as claimed in claim 1, it is characterised in that the removal is molten
The method of agent is to make solvent permeable by the multiple perforate.
9. the preparation method of macroscopical aggregation of micro Nano material as claimed in claim 1, it is characterised in that described micro-nano
Micro-nano unit in unit dispersion liquid forms macroscopical aggregation of micro Nano material after removal of solvents；By the micro-nano material
Macroscopical aggregation of material releases to form a micro Nano material fiber from outlet；While by export side micro Nano material it is grand
See aggregation to extract out, while from the new micro-nano unit dispersion liquid of inlet side injection, continuously prepare micro Nano material
Fiber.
10. the preparation method of macroscopical aggregation of micro Nano material as claimed in claim 1, it is characterised in that when the micro-nano
After micro-nano unit concentration in meter Dan Yuan dispersion liquids reaches certain value, by refrigerating plant by the micro-nano unit dispersion liquid
Freezing forms a precast body；Then after the precast body is taken out, the solvent of residual is removed by distilling, obtains micro Nano material
Macroscopical aggregation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610275584.2A CN105948024B (en) | 2016-04-29 | 2016-04-29 | The preparation method of macroscopical aggregation of micro Nano material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610275584.2A CN105948024B (en) | 2016-04-29 | 2016-04-29 | The preparation method of macroscopical aggregation of micro Nano material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105948024A CN105948024A (en) | 2016-09-21 |
| CN105948024B true CN105948024B (en) | 2018-01-09 |
Family
ID=56916165
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610275584.2A Expired - Fee Related CN105948024B (en) | 2016-04-29 | 2016-04-29 | The preparation method of macroscopical aggregation of micro Nano material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105948024B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107879331A (en) * | 2016-09-29 | 2018-04-06 | 河南烯碳合成材料有限公司 | The method for manufacturing graphene of the basal plane lateral dimensions more than 50 nanometers |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768365A (en) * | 2008-12-29 | 2010-07-07 | 翁文桂 | Polymer composite material with oriented padding and preparation method thereof |
| CN103342351B (en) * | 2013-07-10 | 2015-02-18 | 昆明纳太能源科技有限公司 | Method and device for preparing directionally arranged bucky paper in large scale |
| CN103374690B (en) * | 2013-07-26 | 2015-12-02 | 河南理工大学 | The preparation method of the carbon nanotube/alloy composite materials of carbon nano-tube oriented arrangement |
| CN104876179B (en) * | 2015-04-16 | 2017-01-11 | 华中科技大学 | Large-area assembling method for non-contact type one-dimensional nano material |
-
2016
- 2016-04-29 CN CN201610275584.2A patent/CN105948024B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN105948024A (en) | 2016-09-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Chun et al. | Inertial migration of neutrally buoyant particles in a square duct: An investigation of multiple equilibrium positions | |
| Lee et al. | Microfluidic four-roll mill for all flow types | |
| Nagayama et al. | Effects of interface wettability on microscale flow by molecular dynamics simulation | |
| Jing et al. | Size dependences of hydraulic resistance and heat transfer of fluid flow in elliptical microchannel heat sinks with boundary slip | |
| Shi et al. | Growth of viscoelastic instabilities around linear cylinder arrays | |
| Gudipaty et al. | Cluster formation and growth in microchannel flow of dilute particle suspensions | |
| Luelf et al. | Rope coiling spinning of curled and meandering hollow-fiber membranes | |
| JP2009291783A (en) | Method of sorting particle or cluster of particle in fluid flowing in channel | |
| CN107020054A (en) | A kind of preparation method of the high heat conduction phase-change microcapsule of uniform particle sizes | |
| Devlin et al. | The importance of gravity in droplet evaporation: A comparison of pendant and sessile drop evaporation with particles | |
| CN105948024B (en) | The preparation method of macroscopical aggregation of micro Nano material | |
| CN105712319B (en) | The preparation facilities of macroscopical aggregation of micro Nano material | |
| CN205653167U (en) | Preparation facilities of macroscopical aggregate of little nano -material | |
| Dubov et al. | Regimes of wetting transitions on superhydrophobic textures conditioned by energy of receding contact lines | |
| Yun et al. | Continuous production of solid lipid nanoparticles by liquid flow-focusing and gas displacing method in microchannels | |
| Jiang et al. | Solute transport in two-zone packed tube flow: Long-time asymptotic expansion | |
| Verma et al. | Grain growth stagnation in solid state thin films: A phase-field study | |
| DE102016011540B3 (en) | Vortex tube for separating a fluid flow into two partial streams | |
| Li et al. | Strengthening unidirectional liquid pumping using multi-biomimetic structures | |
| Kurdzinski et al. | Dynamics of high viscosity contrast confluent microfluidic flows | |
| Suroso et al. | Convective heat transfer of nanofluids TiO2/Thermo Oil XT 32 in concentric tube heat exchanger | |
| CN101658734B (en) | The method of splitting fluid flows | |
| Miao et al. | Shape evolution and scaling analysis of soluble cylinders in dissolutive flow | |
| Bhattacharya et al. | Radial distribution and axial dispersion of suspended particles inside a narrow cylinder due to mildly inertial flow | |
| Zheng et al. | Suspended particle motion close to the surface of rotating cylindrical filtering membrane |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180109 Termination date: 20180429 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |