CN106744675B - A kind of nano material cutting off processing method - Google Patents
A kind of nano material cutting off processing method Download PDFInfo
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- CN106744675B CN106744675B CN201710045914.3A CN201710045914A CN106744675B CN 106744675 B CN106744675 B CN 106744675B CN 201710045914 A CN201710045914 A CN 201710045914A CN 106744675 B CN106744675 B CN 106744675B
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- nano material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
- B82B3/0004—Apparatus specially adapted for the manufacture or treatment of nanostructural devices or systems or methods for manufacturing the same
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention relates to nano material processing technique fields, and in particular to a kind of nano material cutting off processing method, including nano material is contacted into Li+Lithiation occurs, then exerts a force to nano material, nano material is made to be broken from lithiumation position and non-lithiumation position intersection, realizes the cut-out to nano material.Nano material cutting-off method of the present invention is that the expansion of nano material lithiumation is made to generate stress effect in the way of lithiumation in situ so that nano material can be broken in the intersection of lithiumation and non-lithiumation by tensile stress or bending stress, complete the cut-out of nano material.The mechanism that it cuts off is related with the lithiumation of nano material, by controlling lithiumation rate and lithiumation time, realize the controllability of nano material lithiumation length, it realizes and the controllable precise that nano material is cut off in the longitudinal direction is processed, and it is not influenced by performances such as rapidoprint thickness, conductive capabilities, it is applied widely, it is easy to operate, it is easily controllable, it is suitable for popularization and application.
Description
Technical field
The present invention relates to nano material processing technique fields, and in particular to a kind of nano material cutting off processing method.
Background technology
Since twentieth century nineties, status of the nano material in scientific research field becomes more and more important.Due to nano material
Performance and its size, pattern it is closely bound up, the controllable preparation of nano material is that nano material synthesis field is always pursued
Important goal.But it finally realizes that the controllable preparation of nano material is still by synthetic method physically or chemically at present and receives
The difficult point of rice field of material preparation, but which greatly limits the further applications of nano material, moreover, at present to growing out
The means that the size and shape of nano material cut again and is interconnected later to them are seldom.
The method of chemical attack and mechanical lapping is the method for common simple processing nano material, but both methods
The length of nano wire can not accurately be controlled, while also defect can be brought to nanotube during grinding.Nano material
Accurate processing is generally required by focused ion beam technology(FIB), scanning electron microscope(SEM), atomic force microscope
(AFM), transmission electron microscope(TEM)Equal tools.Nano material can be accurately processed using FIB and is realized in a certain range
Three-dimension process, but larger damage inevitably is brought to sample in process and introduces pollution of ion source;Profit
The fixed carbon nanotube in both ends can be cut off with the electron beam of SEM, the length to realize carbon nanotube controls, but this
The principle of kind of cutting method is to irradiate during carbon nanotube chemical bond in destroying carbon nanometer tube with electron beam, is not particularly suited for
The diameter material larger compared with thick and chemical bond energy;Can be for the machine cuts of graphene using AFM probe needle point, but cut
In the process can be larger to the abrasion of AFM probe needle point, and cutting efficiency is low(It is limited to the sweep speed of AFM probe), it is desirable that
The thickness of sample of cutting is small(Several nanometers), surface smoothness it is high, be only applicable to cut few layer graphene, few layer MoS2Etc. ultra-thin
Stratified material, refer to that Liu Lianqing, Yu, seat are peaceful etc. entitled to be based on atomic force microscope what Chinese science magazine was delivered
Graphene controllable method of cutting out research paper in record.It is in TEM, two carbon nanotubes are opposite, it is one of to make
For field emission source, carbon nanotube can gradually shorten under Flied emission electric field action;Chinese patent 200610113318.6 discloses
A kind of accurately cut-out and skiving nano material method are using a kind of nano material as nano-knife and to need nanometer to be cut
Material is contacted in the position cut, and cutting to nano material is realized by applying alive mode.However both methods
Determine that they are only applicable to the preferable nano material of electric conductivity in the incision principle of cutting nano material.
Invention content
In order to overcome the deficiencies of existing technologies, nanometer wide, easy to operate that the object of the present invention is to provide a kind of applicabilities
Material cutting off processing method is realized and is processed to the controllable precise of nano material length.
In order to achieve the goal above, the technical solution adopted in the present invention is:
A kind of nano material cutting off processing method, including nano material is contacted into Li+Lithiation occurs, then to nanometer
Material exerts a force, and nano material is made to be broken from lithiumation position and non-lithiumation position intersection, realizes the cut-out to nano material.
Optionally, described that nano material is contacted into Li+Specific method be:Taking being capable of substance that is conductive and providing lithium ion
As anode, nano material as cathode, can material surface conductive and that lithium ion is provided there is solid electrolyte layer, manipulate
Positive contact nanometer material applies voltage in positive and negative end.The control of alive size is applied by control can be conductive and to carry
Li is transmitted to nano material by solid electrolyte for the substance of lithium ion+Rate, control the lithiumation rate of nano material, into
And the alive time is applied by control to control the time of lithiumation, realize the control to lithiumation length, and then realize to nanometer
The controllable precise processing that material is cut off in the longitudinal direction.
Optionally, described is to apply tensile stress or bending stress to nano material to nano material force.
Optionally, the nano material is conductor or semi-conducting material.The electric conductivity of semi-conducting material is not required.
Optionally, the nano material is element semiconductor material, including carbon nanomaterial, graphene nano material, silicon
Nano material or germanium nano material;
Metal oxide semiconductor material, including TiO2Nano material, ZnO nano material, WO3Nano material or SnO2It receives
Rice material;
Metal tungsten sulfide semi-conducting material, including WS2Nano material, MoS2Nano material or ZnS nano materials.
Optionally, the nano material is single nano-wire or nanotube.
The above method is completed in TEM, and concrete operations are:Conductor is inserted into one end of setting-out product in TEM-STM specimen holders
Silk dips on conductor silk and needs cut-off nano material;Then conductor needle point is taken, coating surface has on conductor needle point
Solid electrolyte layer can substance conductive and that lithium ion is provided, conductor needle point is packed into TEM-STM specimen holders, then will
TEM-STM specimen holders are fitted into TEM, and using conductor needle point as anode, conductor silk applies electricity as cathode, anode and cathode both ends
Pressure, manipulates conductor needle point and nano material that the needs that are dipped on conductor silk are cut-off contacts, on conductor needle point can conduction and
The substance of lithium ion is provided by the solid electrolyte on its surface by Li+It is spread to nano material, makes nano material that lithiumation occur
Reaction manipulates conductor needle point and exerts a force to nano material, make to receive in the intersection of lithiumation and non-lithiumation when needing at fracture position
Rice material is broken in the intersection of lithiumation and non-lithiumation, realizes the cut-out to nano material.
Optionally, the operation conductor needle point nano material cut-off with the needs dipped on conductor silk contacts specific
Method is:The end for manipulating the nano material that conductor needle point is cut off with the needs dipped on conductor silk contacts, and makes nano material
Lithiation takes place from an end.
Optionally, the operation conductor needle point nano material cut-off with the needs dipped on conductor silk contacts specific
Method is:It is connect at the position that the needs of the manipulation conductor needle point nano material cut-off with the needs dipped on conductor silk are broken
It touches, makes nano material that lithiation occur from the end direction for needing to give up after cutting off to nano material from the position being broken.
It is above-mentioned during cutting off processing nano material, by applying voltage in positive and negative end, to make a nanometer material in TEM
Negative voltage is presented relative to tungsten tip in material, and control applies the transmission rate of alive size control Li+, controls the lithium of nano material
Change rate, and then apply the time of alive time control lithiumation by control, the final length for controlling lithiumation is realized to nanometer
The controllable precise processing of cutting off processing on length of material direction.
It is above-mentioned in TEM during cutting off processing nano material, specimen holder is electrically connected with TEM in-situ control systems, energy
Enough realize manipulates the movement of conductor needle point and exerts a force to the nano material that need to be cut off, and applies negative voltage to conductor silk.TEM is in situ
Control system includes that scanning probe control unit manipulates that conductor needle point is mobile and force, further include voltage control system control to
Positive and negative anodes apply voltage.
Optionally, the coating surface on conductor needle point have solid electrolyte layer can be conductive and lithium ion is provided
The specific method of object be:Lithium metal is coated on conductor needle point in glove box, conductor needle point is being packed into TEM-STM samples
Bar and by TEM-STM specimen holders be packed into TEM during, lithium metal exposure in air surface be oxidized to form one layer of oxidation
Lithium, this layer of lithia are solid electrolyte layer.
Optionally, the material that the conductor silk uses is gold.
Optionally, the material that the conductor needle point uses is tungsten.
It is found according to correlative study, the negative material of lithium battery is often subject to huge in lithiumation and move back lithiumation during
Big volume expansion/contraction process and cause the intensity of material to decline and even fragmentation phenomenon occur.For example, Si by complete lithiumation at
For Li4Adjoint volume expansion is up to 400% when .4Si, and so violent volume expansion can cause huge in electrode material
Stress effect, the on-spot study in TEM find that the axial rupture strength of Si drops to 0.72 Gpa from 3.6 GPa after lithiumation;.
But in these document reports nano material generated in lithiumation stress and therefrom caused by showing of being substantially reduced of intensity
It needs strongly to avoid when as lithium battery material as being all these materials, be proposed based on this phenomenon without researcher
The processing technology of nano material.Therefore the present invention proposes a kind of new mode to process nano material, is exactly first to nanometer
Material carries out partial lithiation, and lithiumation partial intensities substantially reduce and will appear in the intersection of lithiumation and non-lithiumation larger at this time
Stress, finally applying tensile stress or bending stress, nano material to nano material can send out in the intersection of lithiumation and non-lithiumation
Raw fracture.
Nano material cutting off processing method of the present invention is to cut off nano material in the way of lithiumation in situ, cut-out
Mechanism is related with the lithiumation of nano material, the stress effect for generating nano material after lithiumation so that nano material is by curved
When the effect of transverse stress or tensile stress, lithiumation intersection has been broken in non-lithiumation and, realizes the cut-out to nano material, no
It is influenced by performances such as rapidoprint thickness, it is applied widely, it is easy to operate, it is easily controllable, it is suitable for popularization and application.
Further, nano material cutting off processing method of the present invention, by way of simulating solid lithium battery, by nanometer material
Material is used as cathode, can substance conductive and that lithium ion is provided as positive mode, by Li+It is transmitted to nano material, makes to receive
Lithiumation occurs for rice material, can control Li by way of controlling voltage in this way+Transmission rate, and then control nano material
Lithiumation rate, and then the length of lithiumation is controlled by controlling the time of lithiumation, it realizes and nano material is cut off in length direction
Controllable precise processing.
Further, nano material cutting-off method of the present invention is complete in TEM when being cut off for single nano material
At, image that can be by tem observation nano material during lithiumation, the position of lithiumation is deposited relative to the position of non-lithiumation
In volume expansion, off-position is needed when showing that the intersection of lithiumation and non-lithiumation is in the image for the nano material observed
When place, stops silk applies negative pressure, stops lithiation, applies tensile stress or bending stress to single nano material,
So that single nano material is broken in the intersection of lithiumation and non-lithiumation, the cut-out of single nano material is completed.
Further, in TEM carry out nano material cut-out during, be by positive and negative end apply voltage,
So that negative voltage is presented relative to tungsten tip in nano material so that the lithium ion with positive charge is to the nanometer material with negative voltage
Expect direction movement, realize contact of the lithium ion with nano material, and then make nano material that lithiumation occur, then lithium ion is to nanometer
The performances such as rate of material transfer just influence whether the lithiumation rate of nano material, and the rate that lithium ion is shifted to nano material
It can be influenced again by the size of voltage, voltage is bigger under normal conditions, and the transfer rate of lithium ion is faster, and then nano material
Lithiumation rate it is also faster, therefore the lithiumation rate that alive size controls nano material can be applied by control, from nanometer
When certain one end of material proceeds by lithiumation, the length that lithiumation has occurred can be accurately controlled by way of controlling the lithiumation time
Degree, and then apply stress directly at required position, nano material is cut off, is realized to nano material in the longitudinal direction
The accurate processing of cut-out.
Description of the drawings
Fig. 1 is to dip multi wall WS on spun gold in embodiment2The TEM of nanotube schemes;
Fig. 2 is WS in embodiment2TEM after nanotube is contacted with tungsten tip schemes;
Fig. 3 is WS in embodiment2TEM figure of the nanotube in non-lithiumation and lithiumation intersection fracture;
Fig. 4 is WS in embodiment2The WS of non-lithiumation after nanotube fracture2The TEM of nanotube schemes;
Fig. 5 is WS in embodiment2The WS of lithiumation after nanotube fracture2The TEM of nanotube schemes.
Specific implementation mode
Technical scheme of the present invention is described in detail below by the specific embodiment of the cut-out to single nano-wire.
Following embodiments carry out the cutting of single nano-wire in TEM, and wherein TEM-STM specimen holders are electrically connected with
TEM in-situ control systems, packet scanning probe control system and voltage control system in TEM in-situ control systems;Wherein scanning is visited
Needle control system is used to control the movement of tungsten tip and exerts a force to nano material, and voltage control system is applied for controlling to positive and negative anodes
Making alive.
Embodiment
The present embodiment WS2Nano material cutting off processing method, concrete operation step are:
1)One end of setting-out product is inserted into and takes spun gold in TEM-STM specimen holders, and multi wall WS is dipped on spun gold2Nanotube,
As shown in Figure 1;
2)The tungsten filament NaOH solution of a diameter of 0.2mm is taken to corrode to obtain the tungsten tip that radius of curvature is less than 100 nanometers,
One layer of lithium metal is coated on tungsten tip surface in glove box, tungsten tip is then put into step 1)TEM-STM specimen holders in, so
TEM-STM specimen holders are put into TEM afterwards, the lithium metal with air on tungsten tip surface contact to form one layer of oxidation in the process
Lithium, the WS of this layer of lithia thereafter2Play the role of solid electrolyte during nanotube lithiumation;
3)Spun gold, as cathode, passes through the TEM in-situ controls being electrically connected with TEM-STM specimen holders as anode, tungsten tip
System applies voltage to positive and negative end, and manipulates tungsten tip movement and the WS on spun gold2The end of nanotube contacts, such as Fig. 2
It is shown;Lithium ion Li with positive charge+WS on the spun gold that negative electricity pressure condition is presented2Nanotube diffusion movement so that nanometer
Lithiation in situ, WS occur for pipe2+4Li+→W+Li2S, the nanotube volume expansion 16.1% after lithiumation, when lithiumation and non-lithium
Change intersection positioned at when needing at fracture position, stopping applies voltage to positive and negative end, and manipulating tungsten tip is needing at fracture position
To WS2Nanotube applies bending stress so that WS2Nanotube is broken, as shown in Figure 3;Lithiation does not occur wherein
WS2Nanotube retains original pattern, as shown in Figure 4 and Figure 5, that is, completes to WS2The cut-out of nanotube.
The single nano material of other compositions can also be cut off using the present embodiment the method, such as carbon nanometer material
Material, graphene nano material, silicon nano material, germanium nano material, TiO2Nano material, ZnO nano material, WO3Nano material or
SnO2Nano material, WS2Nano material, MoS2Nano material, ZnS nano materials.
The lithiumation rate of nano material applies voltage swing and nano material the application with operating process to spun gold
Property is related, and for identical material, if other conditions are the same, voltage is bigger, and lithiumation rate is bigger, by detection
Under 2V voltages, the lithiumation rate of different materials is as follows:
The lithiumation speed of Si nano wires is about:0.01nm/s, SnO2The lithiumation speed of nano wire is about 8nm/s, WO3
Nano wire lithiumation speed is about 133nm/s, WS2Nanotube is about 180nm/s.In actual mechanical process, it can pass through
The mode for controlling voltage and lithiumation time, accurately controls the length of nano wire lithiumation, and then accurately control lithiumation and non-lithiumation
Delivery position, and then realize accurate cut-out to nano wire.
From being to control the movement of tungsten tip, the material cut off to needs by TEM in-situ control systems in this present embodiment
Force, and apply voltage to spun gold and tungsten tip both ends, therefore the system determines to nano material the control accuracy of voltage
Cut-out precision.Normal controller can be as accurate as 10ms for control time, and may be only accurate to 0.5s by artificially controlling,
For WS2Nanotube, lithiumation rate are 180nm/s, can be reached by the lithiumation precision of control system computer software control
To 1.8nm, the lithiumation precision by the manual control lithiumation time is 90nm.
Claims (9)
1. a kind of nano material cutting off processing method, which is characterized in that including nano material is contacted Li+Lithiation occurs, so
It exerts a force afterwards to nano material, nano material is made to be broken from lithiumation position and non-lithiumation position intersection, realize to nano material
Cut-out;The nano material is nano wire or nanotube.
2. nano material cutting off processing method as described in claim 1, which is characterized in that described that nano material is contacted Li+'s
Specific method is:Take can substance conductive and that lithium ion is provided as anode, nano material is used as cathode, conduction and can carry
There is solid electrolyte layer for the material surface of lithium ion, manipulate positive contact nanometer material, apply voltage in positive and negative end.
3. nano material cutting off processing method as claimed in claim 2, which is characterized in that the nano material is conductor or half
Conductor material.
4. nano material cutting off processing method as claimed in claim 3, which is characterized in that the method is completed in TEM, tool
Gymnastics conduct:Conductor silk is inserted into one end of setting-out product in TEM-STM specimen holders, is dipped on conductor silk and needs what is be cut off to receive
Rice material;Then take conductor needle point, on conductor needle point coating surface have solid electrolyte layer can be conductive and lithium is provided
Conductor needle point is packed into TEM-STM specimen holders, then TEM-STM specimen holders is fitted into TEM, by conductor needle by the substance of ion
Point is used as anode, conductor silk to apply voltage as cathode, anode and cathode both ends, dipped on manipulation conductor needle point and conductor silk
Cut-off nano material is needed to contact, it being capable of substance conductive and that lithium ion the is provided solid that passes through its surface on conductor needle point
Electrolyte is by Li+It is spread to nano material, makes nano material that lithiation occur, exist in the intersection of lithiumation and non-lithiumation
When needing at fracture position, manipulates conductor needle point and exert a force to nano material, make nano material in the intersection of lithiumation and non-lithiumation
It is broken, realizes the cut-out to nano material.
5. nano material cutting off processing method as claimed in claim 4, which is characterized in that the operation conductor needle point and conductor
The specific method of the cut-off nano material contact of needs dipped on silk is:Manipulate the need dipped on conductor needle point and conductor silk
The end for the nano material to be cut off contacts, and makes nano material that lithiation take place from an end.
6. nano material cutting off processing method as claimed in claim 4, which is characterized in that the operation conductor needle point and conductor
The specific method of the cut-off nano material contact of needs dipped on silk is:Manipulate the need dipped on conductor needle point and conductor silk
It is contacted at the position that the needs for the nano material to be cut off are broken, makes nano material from the position for needing to be broken to nanometer material
Lithiation occurs for the end direction given up after material cut-out.
7. nano material cutting off processing method as claimed in claim 4, which is characterized in that described to coat table on conductor needle point
There is the specific method for capableing of substance that is conductive and providing lithium ion of solid electrolyte layer to be in face:In conductor needle in glove box
Lithium metal is coated on point, during being packed into TEM-STM specimen holders by conductor needle point and TEM-STM specimen holders be packed into TEM,
Lithium metal exposure is oxidized to form one layer of lithia in surface in air, this layer of lithia is solid electrolyte layer.
8. nano material cutting off processing method as claimed in claim 4, which is characterized in that the material that the conductor silk uses for
Gold.
9. nano material cutting off processing method as claimed in claim 4, which is characterized in that the material that the conductor needle point uses
For tungsten.
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