CN100411742C - Mechanically shearing process of preparing one-dimensional nanometer material - Google Patents
Mechanically shearing process of preparing one-dimensional nanometer material Download PDFInfo
- Publication number
- CN100411742C CN100411742C CNB2006101175808A CN200610117580A CN100411742C CN 100411742 C CN100411742 C CN 100411742C CN B2006101175808 A CNB2006101175808 A CN B2006101175808A CN 200610117580 A CN200610117580 A CN 200610117580A CN 100411742 C CN100411742 C CN 100411742C
- Authority
- CN
- China
- Prior art keywords
- nanometer material
- monodimension nanometer
- shearing
- mechanical shearing
- superabrasive particle
- 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
Images
Abstract
The present invention relates to nanometer material processing technology, and is especially mechanically shearing process of preparing one-dimensional nanometer material. The mechanically shearing process of preparing one-dimensional nanometer material with superhard particle includes the steps of: forming mechanical shearing tool, shearing one-dimensional nanometer material and separating the one-dimensional nanometer material from the mechanical shearing tool. The mechanical shearing tool may be one metal plane with adhered superhard particle or grown superhard particle, one edged roller with adhered superhard particle or superhard particle mixed directly with the material to be processed. By means of selecting superhard particle, short one-dimensional nanometer material of length from several hundred nanometer to several microns may be obtained. The short one-dimensional nanometer material is easy to disperse in solid or liquid medium.
Description
Technical field
The present invention relates to a kind of method of nano material processing technique field, specifically is a kind of method of mechanical shearing monodimension nanometer material.
Background technology
Monodimension nanometer materials such as CNT have many superior functions, can be applicable to multiple fields such as electronics, machinery, the energy, material, and the application facet at nanometer electronic device and super composite has great potential especially.But monodimension nanometer materials such as the CNT of preparing usually have bigger specific area and higher draw ratio, very easily reunite and winding mutually, are difficult to dispersion and handle.If be cut into short monodimension nanometer material then difficult the winding, how evenly dispersion in solid phase or liquid phase medium easily is so effectively to cut short a key technology that is processed in its application process to monodimension nanometer materials such as long CNTs.
So far, the existing method that monodimension nanometer materials such as CNT are sheared relates generally to chemical attack or physical grinding process.Wherein, with strong oxidizer oxidations such as concentrated acid or nitration mixture, nickel catalytic oxidation, fluoridize the fault of construction that chemical methodes such as heat treatment depend on monodimension nanometer materials such as CNT strongly, cause the control of sheared length and difficult quality, structural deterioration to monodimension nanometer materials such as CNTs is bigger, is not suitable for using on a large scale.Physical method mainly comprises and CNT directly carried out ball milling and with certain additive ball milling, these class methods do not rely on the character of CNT itself, and can carry out fairly large production, therefore obtained paying close attention to widely.
Find through literature search prior art, " Segmented and opened multi-walled carbonnanotubes " (shearing of multi-walled carbon nano-tubes and the opening) that G.Maurin etc. deliver on " Carbon " (carbon) calendar year 2001 the 39th volume 1273-1278, this article proposes the method for direct ball milling truncating carbon nano-tubes, concrete grammar is: CNT is dispersed in the ethanol, and the disk that utilizes the surface to coat diamond dust volatilizees up to ethanol to mill.Its deficiency is: the time of grinding is long, and because the repeatedly collision of diamond dust and CNT causes the tube wall of CNT to be subjected to very big destruction.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of mechanical shearing method of rapidly and efficiently cutting short monodimension nanometer materials such as CNT is provided, i.e. the method for mechanical shearing monodimension nanometer material can obtain length and be the hundreds of nanometer to several microns long monodimension nanometer material.
The present invention is achieved by the following technical solutions, and the present invention adopts superabrasive particle to realize the mechanical shearing monodimension nanometer material, and concrete processing step comprises:
(1) forms the cutting implement that mechanical shearing needs, be in shearing blade, knife edge board and the blade roller bearing any one;
(2) shearing of monodimension nanometer material;
(3) monodimension nanometer material and mechanical shearing instrument separates.
The cutting implement that formation mechanical shearing of the present invention needs, can adopt following method to realize:, the preparation method of knife edge board comprises that the superabrasive particle that will prepare is bonded on the flat board; Or at metal plate surface direct growth superabrasive particle; The preparation method of blade roller bearing is included in roller surface bonding superabrasive particle; The third is directly to use shearing blade that monodimension nanometer material is sheared, and does not promptly use binding agent, directly monodimension nanometer material is mixed with superabrasive particle.
The shearing of monodimension nanometer material of the present invention, detailed process is as follows: a certain amount of monodimension nanometer material is put between two above-mentioned knife edge boards, then two knife edge boards are applied certain pressure, under the effect of shear stress, superabrasive particle carries out machine cuts to monodimension nanometer material, thereby realizes blocking of monodimension nanometer material.Perhaps a certain amount of monodimension nanometer material is put into continuously between the above-mentioned blade roller bearing of two rollings, under the effect of shear stress, superabrasive particle carries out machine cuts to monodimension nanometer material, monodimension nanometer material after the shearing falls and is collected or is adsorbed on roller surface, thereby realizes the continued operation that nano material is blocked.Perhaps directly the superabrasive particle accumulation horizon that is mixed with monodimension nanometer material is exerted pressure, superabrasive particle carries out machine cuts to monodimension nanometer material, thereby realizes the brachymemma of monodimension nanometer material.
Monodimension nanometer material of the present invention separates with cutting implement, detailed process is as follows: it is ultrasonic and centrifugal that the mixture of the knife edge board behind the mechanical shearing or shearing blade and monodimension nanometer material is put into certain medium, and the shearing monodimension nanometer material that adheres to is separated with cutting implement.It is ultrasonic and centrifugal that the monodimension nanometer material of collecting after perhaps will being sheared by the blade roller bearing is put into certain medium, and monodimension nanometer material is separated with the superabrasive particle that comes off.
Adhesive method described in the present invention comprises electrostatic sand-planting and adopts binding agent to paste.
Binding agent described in the present invention comprises polyamide curing agent, phenolic resins, epoxy resin etc.
Superabrasive particle described in the present invention comprises monocrystalline, polycrystalline and the particle of hardness higher (Rockwell hardness is greater than 90), and material mainly comprises diamond, carborundum, corundum, quartz etc.
Monodimension nanometer material of the present invention comprises single wall and multi-walled carbon nano-tubes, carbon nano-fiber, silicon nanowires, silicon carbide whisker, metal oxide nano band and metal oxide nanotubes etc.
Medium of the present invention comprises water, ethanol, acetone, isopropyl alcohol equal solvent.
Compared with the prior art the present invention has following characteristics: the shear efficiency height of monodimension nanometer material; Do not have the repeated impact in the physics modes such as grinding, structural deterioration in the shear history and damage are less; Can realize the continuous production of shearing when adopting blade roller bearing mode to carry out mechanical shearing; The present invention is specially adapted to the process technology of cutting short of single wall and monodimension nanometer materials such as multi-walled carbon nano-tubes, carbon nano-fiber, silicon nanowires, silicon carbide whisker, metal oxide nano band and pipe.
Description of drawings
Fig. 1 knife edge board cut mode work schematic diagram
Fig. 2 blade roller bearing cut mode work schematic diagram
After disperseing, Fig. 3 carbon nanometer tube material drops in the SEM photo on the silicon chip in ethanol
After disperseing, CNT after Fig. 4 embodiment 1 shears drops in the SEM photo on the silicon chip in ethanol
After disperseing, CNT after Fig. 5 embodiment 2 shears drops in the SEM photo on the silicon chip in ethanol
The specific embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
The preparation of described superabrasive particle knife edge board of present embodiment or roller bearing, specifically can adopt following measure:
(1) be coated with a layer binder on paper, cloth or metal polar plate, bondline thickness is 0.02-0.5mm.Superabrasive particle evenly is sprinkling upon on the binding agent, and diameter of particle is 1-12 μ m.At 30-60 ℃ of dry 0.5-4 hour, form the superabrasive particle knife edge board that needs, i.e. sand paper or emery cloth then.
(2) mode that adopts chemical vapor-phase growing (CVD) is at substrate surface growth one deck superabrasive particle film, and particle size is 0.1-12 μ m, forms the superabrasive particle knife edge board that needs.
(3) directly monodimension nanometer material is sneaked into superabrasive particle, the superabrasive particle accumulation horizon that is mixed with monodimension nanometer material is exerted pressure, particle size is 0.1-12 μ m, forms the superabrasive particle knife edge board that needs.
(4) be coated with a layer binder in the metal roller surface, bondline thickness is 0.02-0.5mm.Superabrasive particle evenly is sprinkling upon on the binding agent, and diameter of particle is 1-12 μ m.At 30-60 ℃ of dry 0.5-4 hour, form the superabrasive particle blade roller bearing that needs then.
The shearing of the described CNT of present embodiment and separation process are: a pair of centre is placed with two-sided the exerting pressure of superabrasive particle knife edge board of CNT, and the pressure size is 10-100Mpa.Then above-mentioned superabrasive particle knife edge board was put into water etc. the ultrasonic 1-10 of medium minute, ultrasonic power is the 1-5 watt.Take out the superabrasive particle knife edge board, the further ultrasonic even carbon nanotube that makes disperses to form suspension, and ultrasonic power is the 10-100 watt, and ultrasonic time is 5-30 minute.Suspension is carried out centrifugation, and centrifugal rotational speed is 100-2000 rev/min, and centrifugation time is 5-15 minute, gets the short carbon nanometer tube that upper strata suspension liquid drying can obtain high dispersive.Perhaps adjust two distances between the above-mentioned blade roller bearing, make two pressure between the blade roller bearing at 10-50MPa, CNT is put into continuously between the roller bearing of two rotations, the monodimension nanometer material that falls was collected and put into water etc. the ultrasonic 5-30 of medium minute, ultrasonic power is the 10-100 watt.Suspension is carried out centrifugation, and centrifugal rotational speed is 100-2000 rev/min, and centrifugation time is 5-15 minute, gets the short monodimension nanometer material that upper strata suspension liquid drying can obtain high dispersive.
Further each embodiment is elaborated below:
Embodiment 1
Utilize the carborundum paper of buying (the sand grains diameter is the 2-4 micron) as the shearing knife edge plate, CNT to be placed on the sand paper, two sides sand paper utilizes powder compressing machine that it is exerted pressure to putting and put into the mould of a fixed structure, and pressuring method as shown in Figure 1.Pressure is 40MPa, and be 2 minutes pressing time.Take out sand paper then, put into water and carry out ultrasonicly, take out sand paper behind the ultrasonic 5min.The aqueous solution that contains CNT is carried out centrifugal 5min, and rotating speed is 100 rev/mins.Extract top suspension, drying can obtain short CNT.The raw material that Fig. 3 uses for this embodiment, the length of CNT is longer, and twines mutually.The scanned photograph of the short carbon nanometer tube that Fig. 4 finally obtains for this embodiment is compared with raw material, and CNT obviously shortens, and average length and can be in ethanol be evenly disperseed about 500nm.
Embodiment 2
Matrix paper or cloth evenly are coated with last layer AG-80 epoxy resin, and bondline thickness is 0.05-0.1mm, sprinkles diadust (diameter is the 1-2 micron) then, at the flat board of 40 ℃ of oven dry preparation in 1 hour diamond coating.Put into the pressure 1 minute of the after-applied 30MPa of CNT.After diamond is removed in centrifugation, can obtain the CNT that average length is 400nm, see shown in Figure 5.
Embodiment 3
Utilize the method for embodiment 2, at diameter is that 5 centimetres roller bearing is pasted one deck diadust and prepared the blade roller bearing that diamond coats, the spacing of adjusting two roller bearings is 4.9 centimetres, and relatively rotate, CNT is fallen slowly, process schematic representation as shown in Figure 2, the length of the CNT after obtaining shearing is 500nm.
Embodiment 4
Utilize the CVD method to prepare the diamond thin of one deck crystal grain diameter for 100-200nm at planar surface, CNT is put into two growths to be had between the substrate of diamond thin, applies 100MPa pressure 2 minutes.Pole plate is put into the ultrasonic 10min of ethanol CNT and diamond thin are broken away from, even carbon nanotube is dispersed in the ethanol carrying out ultrasonic 20min.Centrifugal 10min under 1000 rev/mins rotating speed gets upper strata suspension, and drying can obtain the short carbon nanometer tube that length is 200nm.
Embodiment 5
Put into the diadust (granularity is the 10-12 micron) that is mingled with CNT between two-layer flat board, apply the pressure 2 minutes of 50MPa, centrifugal and the method for separating be with embodiment 1, can obtain length and be 1.5 microns CNT.
Embodiment 6
Use the method for embodiment 2, adopt carborundum (granularity is the 5-7 micron) as superabrasive particle, the length of the CNT that obtains is 900nm.
Embodiment 7
Utilize the aluminum oxide sandpaper of buying (the sand grains diameter is the 10-12 micron) as the shearing knife edge plate, carbon fiber to be placed on the sand paper, two sides sand paper is to putting and apply the pressure of 10MPa, and be 60 seconds pressing time.Take out sand paper then, put into water and carry out ultrasonicly, take out sand paper behind the ultrasonic 5min.The aqueous solution that contains CNT is carried out centrifugal 2min, and rotating speed is 100 rev/mins.The length that obtains carbon fiber is 5 microns.
Claims (9)
1. the method for a mechanical shearing monodimension nanometer material is characterized in that: adopt superabrasive particle to realize the mechanical shearing monodimension nanometer material, concrete steps comprise:
(1) forms the cutting implement that mechanical shearing needs, be in shearing blade, knife edge board and the blade roller bearing any one;
(2) shearing of monodimension nanometer material;
(3) monodimension nanometer material and mechanical shearing instrument separates;
The cutting implement that described formation mechanical shearing needs, can adopt following method to realize: the method that forms knife edge board comprises: the superabrasive particle for preparing is bonded on the flat board, or at metal plate surface direct growth superabrasive particle; The method that forms the blade roller bearing is at roller surface bonding superabrasive particle; The third is directly to use shearing blade that monodimension nanometer material is sheared, and does not promptly use binding agent, directly monodimension nanometer material is mixed with superabrasive particle.
2. the method for mechanical shearing monodimension nanometer material according to claim 1, it is characterized in that, the shearing of described monodimension nanometer material, detailed process is as follows: monodimension nanometer material is put between two above-mentioned knife edge boards, then two knife edge boards are exerted pressure, under the effect of shear stress, superabrasive particle carries out machine cuts to monodimension nanometer material, thereby realizes blocking of monodimension nanometer material; Perhaps monodimension nanometer material is put into continuously between the above-mentioned blade roller bearing of two rollings, under the effect of shear stress, superabrasive particle carries out machine cuts to monodimension nanometer material, monodimension nanometer material after the shearing falls and is collected or is adsorbed on roller surface, thereby realizes the continued operation that nano material is blocked; Perhaps directly the superabrasive particle accumulation horizon that is mixed with monodimension nanometer material is exerted pressure, superabrasive particle carries out machine cuts to monodimension nanometer material, thereby realizes the brachymemma of monodimension nanometer material.
3. the method for mechanical shearing monodimension nanometer material according to claim 2 is characterized in that, described monodimension nanometer material adopts knife edge board or shearing blade to shear, and the described scope of exerting pressure is 10Mpa to 100MPa.
4. the method for mechanical shearing monodimension nanometer material according to claim 1, it is characterized in that, described monodimension nanometer material separates with cutting implement, detailed process is as follows: it is ultrasonic and centrifugal that the mixture of the knife edge board behind the mechanical shearing or shearing blade and monodimension nanometer material is put into medium, and the shearing monodimension nanometer material that adheres to is separated with cutting implement; It is ultrasonic and centrifugal that the monodimension nanometer material of collecting after perhaps will being sheared by the blade roller bearing is put into medium, and monodimension nanometer material is separated with the superabrasive particle that comes off.
5. the method for mechanical shearing monodimension nanometer material according to claim 4 is characterized in that, described medium comprises a kind of in water, ethanol, acetone, the isopropyl alcohol.
6. the method for mechanical shearing monodimension nanometer material according to claim 1 is characterized in that, the bonding described in the method for formation shearing blade and blade roller bearing, its method are electrostatic sand-planting or adopt binding agent to paste.
7. the method for mechanical shearing monodimension nanometer material according to claim 6 is characterized in that, described binding agent comprises a kind of in polyamide curing agent, phenolic resins, the epoxy resin.
8. the method for mechanical shearing monodimension nanometer material according to claim 1 is characterized in that, described superabrasive particle is in diamond, carborundum, corundum, the quartz any one, and the superabrasive particle particle size range is 0.5-12 μ m.
9. the method for mechanical shearing monodimension nanometer material according to claim 1, it is characterized in that, described monodimension nanometer material, a kind of in single wall and multi-walled carbon nano-tubes, carbon nano-fiber, silicon nanowires, silicon carbide whisker, metal oxide nano band and the metal oxide nanotubes.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2006101175808A CN100411742C (en) | 2006-10-26 | 2006-10-26 | Mechanically shearing process of preparing one-dimensional nanometer material |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2006101175808A CN100411742C (en) | 2006-10-26 | 2006-10-26 | Mechanically shearing process of preparing one-dimensional nanometer material |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1974020A CN1974020A (en) | 2007-06-06 |
CN100411742C true CN100411742C (en) | 2008-08-20 |
Family
ID=38124537
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNB2006101175808A Expired - Fee Related CN100411742C (en) | 2006-10-26 | 2006-10-26 | Mechanically shearing process of preparing one-dimensional nanometer material |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN100411742C (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101811662B (en) * | 2010-03-12 | 2013-05-29 | 北京大学 | Method for preparing small-size optical microcavities |
CN106735164B (en) * | 2016-12-08 | 2019-01-25 | 国家纳米科学中心 | The low-dimensional method of nano wire |
CN107324320A (en) * | 2017-07-10 | 2017-11-07 | 安徽理工大学 | A kind of method that mechanical shearing prepares two-dimension nano materials |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20020069505A1 (en) * | 2000-12-07 | 2002-06-13 | Yoshikazu Nakayama And Daiken Chemical Co., Ltd. | Nanotube cartridge and a method for manufacturing the same |
CN1600683A (en) * | 2004-10-26 | 2005-03-30 | 中国科学院长春应用化学研究所 | Method for preparing material of nano carbon tube |
CN1696052A (en) * | 2004-05-10 | 2005-11-16 | 华东理工大学 | Method for preparing Nano carbon tubes |
CN1807233A (en) * | 2006-01-26 | 2006-07-26 | 上海交通大学 | Chemical shearing method for preparing high dispersion short carbon nanometer tube |
-
2006
- 2006-10-26 CN CNB2006101175808A patent/CN100411742C/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20020069505A1 (en) * | 2000-12-07 | 2002-06-13 | Yoshikazu Nakayama And Daiken Chemical Co., Ltd. | Nanotube cartridge and a method for manufacturing the same |
CN1696052A (en) * | 2004-05-10 | 2005-11-16 | 华东理工大学 | Method for preparing Nano carbon tubes |
CN1600683A (en) * | 2004-10-26 | 2005-03-30 | 中国科学院长春应用化学研究所 | Method for preparing material of nano carbon tube |
CN1807233A (en) * | 2006-01-26 | 2006-07-26 | 上海交通大学 | Chemical shearing method for preparing high dispersion short carbon nanometer tube |
Non-Patent Citations (6)
Title |
---|
Segmented and opened multi-walled carbon nanotubes. G. Maurin et al.CARBON,Vol.39 No.8. 2001 |
Segmented and opened multi-walled carbon nanotubes. G. Maurin et al.CARBON,Vol.39 No.8. 2001 * |
碳纳米管的剪切研究. 孙晓刚等.化工新型材料,第33卷第11期. 2005 |
碳纳米管的剪切研究. 孙晓刚等.化工新型材料,第33卷第11期. 2005 * |
碳纳米管的操纵和剪切. 张宇军等.科学通报,第47卷第14期. 2002 |
碳纳米管的操纵和剪切. 张宇军等.科学通报,第47卷第14期. 2002 * |
Also Published As
Publication number | Publication date |
---|---|
CN1974020A (en) | 2007-06-06 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN101980836B (en) | Method and device for forming aggregate abrasive grains for abrading or cutting tools production | |
CN107151001A (en) | A kind of method for preparing high-quality large scale two-dimensional material | |
KR100807450B1 (en) | Polycrystalline abrasive grit | |
CN108349068A (en) | Bonded abrasive article and preparation method thereof | |
CN100411742C (en) | Mechanically shearing process of preparing one-dimensional nanometer material | |
CN104819876B (en) | A kind of film sample preparation method for transmission electron microscope original position added electric field and stress | |
CN107226476A (en) | Two-dimensional thin-layer material coated on surface of microsphere and simple stripping method thereof | |
TW201024034A (en) | Bonded abrasive tool and method of forming | |
CN104803363A (en) | Method for preparing hexagonal boron nitride nanosheets massively | |
CN107298440A (en) | A kind of utilization supercritical fluid continuous method for preparing graphene in screw machine | |
US7141086B2 (en) | Abrasive grain and method for producing it, polishing tool and method for producing it, grinding wheel and method for producing it, and polishing apparatus | |
CN106276881B (en) | A kind of preparation method of graphene | |
CN107163297A (en) | A kind of method that high efficiency prepares the graphene nano sheet material being dispersed in natural polysaccharide | |
CN105950114B (en) | A kind of outer membrane mixing diamond spherical abrasive material and preparation method thereof | |
CN205205070U (en) | Superhard grit and abrasive machining instrument | |
CN103132048A (en) | A polycrystalline diamond grinding material and preparation method for chemical vapor deposition (CVD) | |
JPH0615571A (en) | Abrasive material | |
CN107324320A (en) | A kind of method that mechanical shearing prepares two-dimension nano materials | |
WO2015088807A1 (en) | Polycrystalline compacts, earth-boring tools including such compacts, and methods of fabricating polycrystalline compacts | |
CN105586005B (en) | A kind of preparation method of Nano Alumina Abrasive | |
CN106582449A (en) | Polycrystalline diamond and preparing method and application thereof | |
CN106564889A (en) | Complete equipment for preparing graphene material by means of liquid-state grinding and application thereof | |
CN106865530B (en) | A kind of method that removing prepares the high-speed mixer of graphene and its removes graphene | |
CA2472332C (en) | Method of making a tool component | |
CN202498454U (en) | Abrasive disc for flexible grinding tool |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
C17 | Cessation of patent right | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080820 Termination date: 20111026 |