CN103723672A - Device containing nano-pipet and fabrication method thereof - Google Patents
Device containing nano-pipet and fabrication method thereof Download PDFInfo
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- CN103723672A CN103723672A CN201310477529.8A CN201310477529A CN103723672A CN 103723672 A CN103723672 A CN 103723672A CN 201310477529 A CN201310477529 A CN 201310477529A CN 103723672 A CN103723672 A CN 103723672A
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Abstract
The invention refers to a device containing nano-pipet and a fabrication method thereof. A hollow high aspect ratio sample (such as a nano-test-tube), with a tip that is closed off is secured in a particle beam device (such as a transmission electron microscope). The tip is engaged with the particle beam of the particle beam device until a hole opens up on the tip, thereby turning the high aspect ratio sample into a nano-pipet. Alternatively, a nano-pipet having a hole that does not meet desired parameter values is secured in a particle beam device. The nano-pipet is engaged with the particle beam to attain the desired values of the hole parameters.
Description
Technical field
The present invention relates to produce the nanostructured of molecular scale impact.Specifically, the present invention relates to the device that comprises little opening (for example nanometer pipette (nano-pipet)).
Summary of the invention
For example, by thering is the most advanced and sophisticated hollow high aspect ratio sample (, nanometer test tube) of sealing, be for example fixed on, in beam apparatus (transmission electron microscope).Described tip is contacted with the particle beams of described beam apparatus, until form perforate on described tip, thus described high aspect ratio sample is transformed into nanometer pipette.
The nanometer pipette with the hole of the parameter value that do not meet the expectation is for example fixed on, in beam apparatus (transmission electron microscope).Described nanometer pipette is contacted, to obtain the desired value of hole parameter with the particle beams of described beam apparatus.
Accompanying drawing explanation
From the specific embodiment and accompanying drawing, these and other characteristic of the present invention will become apparent, and these accompanying drawings are:
Fig. 1 illustrates according to the schematic sectional view of the hollow high aspect ratio sample of an embodiment of the present disclosure;
Fig. 2 be by transmission electron microscope, taken according to the tapering part of the hollow high aspect ratio sample of an embodiment of the present disclosure and most advanced and sophisticated photo;
Fig. 3 A-3B is for from manufacture the schematically showing of beam apparatus of nanometer pipette according to the hollow high aspect ratio sample of an embodiment of the present disclosure; And
Fig. 4 is the tapering part of nanometer pipette and the photo in hole of the manufacturing of being taken by transmission electron microscope.
The specific embodiment
The accurate diameter hole of nanometer test tube (being commonly referred to nanometer pipette) end is applied to the various aspects in physics, biology, chemistry and other field.For example, nanometer pipette can be for DNA sequencing.For discriminate individuals molecule, the size of nanometer pipette hole or opening should narrow down to 10 nanometers (nm) below scope.Can repeatedly produce controlled hole size is down to the technique of the nanometer pipette of nanometer range and can be used for many application.
Various embodiments of the present invention instruction nanometer pipette is manufactured.Various embodiments of the present invention allow repeatedly to produce nanometer pipette hole or the opening for example, with required accurate feature (bore dia).Real Time Observation hole characteristic or parameter during manufacture, and during processing, apply them as feedback.Each embodiment instructs and uses beam apparatus (PBD) (that is, using the particle beams of PBD) for example, to form perforate in the tip of high aspect ratio (HAR) sample (, nanometer test tube).Certainly, also can adopt existing nanometer pipette and revise hole.
Fig. 1 illustrates according to the schematic sectional view of the hollow HAR sample of an embodiment of the present disclosure.This hollow HAR sample 10 can be as apply the starting point of the step of disclosure embodiment in manufacturing nanometer pipette.As the waveform dotted line indication in figure, hollow HAR sample can have very long uniform parts, and this part does not need to be shown specifically.Hollow HAR sample 10 has the tapering part 21 stopping at most advanced and sophisticated 31 places.The length of hollow HAR sample 10 can be the arbitrary value between about 1 millimeter to 15 centimetres, but conventionally between 1 centimetre and 3 centimetres.
The cross section of hollow HAR sample normally circular (but not necessarily circular).Hollow HAR sample 10 has the tip 31 in the end sealing of tapering part 21.Term tapering part not meaning that with ways to restrain is understood.Whole hollow HAR sample may be taper, or taper may be so short to such an extent as in fact cannot separate with cusp field.
In an exemplary embodiments of the present invention, most advanced and sophisticated 31 can be very sharp-pointed, in the scope of several nanometers, and may be the highest in the scope of 30 nanometers.The tip 31 of tapering part 21 can characterize by most advanced and sophisticated parameter, and these parameters can be near wall thickness 42 and the point angles 43 of the hollow HAR sample 10 tip 31, and point angle 43 is the tolerance of taper degree.Wall thickness 42 can be crossed over and be worth widely scope.Wall thickness 42 may diminish to 0.5 nanometer, arrives greatly micrometer range.Thin hatching in figure is only intended to the empty space of the hollow HAR sample interior of mark.The nanometer pipette that described hollow HAR sample can be regarded as not being completed into, difference is that nanometer pipette has hole at its most advanced and sophisticated place.
In exemplary embodiment of the present disclosure, hollow HAR sample can be made by drawn glass or other material based on quartzy.Fig. 2 be by transmission electron microscope, taken according to the tapering part of the hollow HAR sample of an embodiment of the present disclosure and most advanced and sophisticated photo.In many cases, also, as in Fig. 2, hollow HAR sample is nanometer test tube.In some cases, this nanometer test tube can have its purposes, and manufactures in some way for use in these possible purposes.From the angle of an exemplary embodiments of the present invention, this nanometer test tube is regarded as manufacturing the parts of nanometer pipette.Tapering part 21, tip 31 and most advanced and sophisticated parameter wall thickness 42 and point angle 43 are indicated in Fig. 1.Give the scale of photo, show the size to most advanced and sophisticated relevant nanometer range.The most shallow shade at hollow HAR sample photo center is the inner surface ripple of test tube, for exemplary embodiment of the present disclosure, there is no special significance.
Fig. 3 A-3B is for from manufacture the schematically showing of beam apparatus of nanometer pipette according to the hollow high aspect ratio sample of an embodiment of the present disclosure.
Fig. 3 A illustrates the initial period that nanometer pipette is manufactured.In the drawings, hollow HAR sample 10 is shown as taper, conventionally towards most advanced and sophisticated 31 end.By sample fixer 103, hollow HAR sample is fixed to (that is, being firmly held in place).Disclose this in the situation that not needing previously to revise hollow HAR sample, PBD sample fixer that can fixation hollow HAR sample 10.In the 13/629th of submission on September 27th, 2012, the sample fixer for fixation hollow HAR sample 10 is disclosed in No. 193 U.S. Patent applications (being all incorporated herein by reference at this).
Hollow HAR sample 10 is in the inside of PBD100.Fig. 3 A-3B only symbolically illustrates PBD100, because have the much this affiliated known equipment of technical field, their details is unimportant.In exemplary embodiment of the present disclosure, PBD can be transmission electron microscope (TEM).But, should be appreciated that, this is only example, and various embodiments of the present invention can be applicable to other PBD, for example SEM (SEM) or FIB (FIB) system.
In PBD inside, the controlled particle beams 102 in such position: PBD can contact with the tip 31 of hollow HAR sample hollow HAR sample 10.Realize with this contact by form the exposure parameter of perforate 11 on most advanced and sophisticated 31 of the particle beams 102, change hollow HAR sample 10 into nanometer pipette 101 thus, as shown in Figure 3 B.
The exposure parameter that is used to form the controlled particle beams 102 of perforate 11 can comprise the duration of particle beams intensity, beam diameter, contact also may comprise other parameter.
In exemplary embodiment of the present disclosure, the contact particle beams 102 is electron beams.Use electron beam, in TEM or SEM, can also for example, to most advanced and sophisticated 31 imagings, as shown in Figure 2.This imaging can be before producing hole, between and carry out afterwards.By this imaging, can obtain most advanced and sophisticated parameter, for example the wall thickness 42 of by the agency of and point angle 43.Described most advanced and sophisticated parameter can be used for optimizing exposure parameter.Use the exposure parameter after optimizing, can obtain the desired value of hole parameter.Can there is many and various holes parameter, specifically depend on the desired use of nanometer pipette, but these parameters generally include the smoothness of the periphery in bore dia, hole, and the shape of the periphery in hole.
In exemplary embodiment of the present disclosure, PBD is TEM, and hollow HAR sample is the nanometer test tube of being made by drawn glass.Various embodiments of the present invention allow to realize high accuracy and repeatability in the manufacture of nanometer pipette.This is due to due to following ability: before the forming process of hole, in and afterwards to sample imaging, and do not need sample to remove or even from sample fixer, remove from PBD.Be used to form the same a branch of also for imaging of hole, this provides essential parameter with a branch of for the hole after optimizing.In order to realize even higher repeatability and hole uniformity, if after bundle contact is with generation hole 11, hole parameter is not desired value, can repeat contact processes by the particle beams 102, until obtain the desired value of hole parameter.
In alternative of the present disclosure, can be from nanometer pipette, this nanometer pipette can produce by any method, and its hole parameter has the value that is different from parameter desired value.Then can make this nanometer pipette contact with the particle beams of PBD so that revaluate more, and obtain the hole parameter value of expectation.
The typical exposure parameter of the electron beam in TEM can be at 30 kilovolts to 400 kilovolt range, and beam electronic current is for receiving ampere to micromicroampere, and beam diameter in 1 nanometer with down to surpassing in the scope of 1000 nanometers, conventionally conform to the size at tip 31.May be as little to several seconds (may be 5 seconds) representative time of contact, mostly is a few minutes most, but is conventionally no more than 1 minute.
Fig. 3 category-B is similar to Fig. 3 A, but the terminal stage that nanometer pipette is manufactured is shown, and has formed hole 11, and hollow HAR sample 10 is transformed into nanometer pipette 101.In this stage, can in imaging, contact the particle beams 102, to guarantee the quality of nanometer pipette 101.
For hole, form, the main effect of postulated particle bundle 102 contacts is 31 regions, tip of the hollow HAR sample 10 of heating.But the environmental condition 110 of PBD inside also can affect hole production process.Environmental condition 110 may affect the degree of heat that the particle beams 102 causes, and environmental condition 110 also may affect hole by chemical effect and form.Under any circumstance, in exemplary embodiment of the present disclosure, in the mode that promotes hole to form, select the environmental condition 110 of PBD100 inside.
That on purpose selects can comprise gas pressure scope for realizing the environmental condition 110 of the PBD100 inside of best hole formation.This pressure limit can be chosen as about 10
-3holder and 10
-7between holder, but conventionally about 10
-4holder and 10
-5between holder.When meeting the pressure limit of selection, can also select to be present in the precursor gases of PBD inside.Can from oxygen-containing gas or hydrogen-containing gas or Halogen gas and composition thereof, select the precursor gases that forms or revise for hole.
Fig. 4 is the tapering part 21 of nanometer pipette 101 and the photo in hole 11 of the method manufacturing of the use exemplary embodiments of the present invention of being taken by transmission electron microscope.Give the scale of photo, to show the sizes related of nanometer pipette 101 devices.Photo demonstration forms horn-like with typical case and unique mode by the periphery in hole 15.This flare is launched to indicate the method that is used to form hole 11.This flare is launched to affect the capillary attribute of nanometer pipette 101, and has useful application, such as but not limited to impact, passes through the flow rate of nanometer pipette 101.
In superincumbent description, with reference to specific embodiment, the present invention has been described.But person of an ordinary skill in the technical field will understand, can carry out various modifications and change, and not depart from the scope of the present invention providing in claim below.Therefore, description and accompanying drawing are regarded as exemplary rather than restrictive, and all such modifications are intended to be included within the scope of the invention.
In addition, any specified material of any structure described here or any appointment size only as an example, are not intended to limit.In addition, if person of ordinary skill in the field is by understanding, can form in the same manner or use structure described here, and with their position and orientation independent.Therefore, to understand, such as " ... below ", " ... above ", " on ... side ", " ... on ", " ... under ", the term of " parallel ", " quadrature ", " vertically " and so on and phrase as used herein, refer to that the each several part of structure is for the relative position of each other and direction, and it is essential or need to be with respect to any specific absolute direction of exterior object to be not intended to hint.
Description above has also been described treatment step.To understand, the order of these steps in different embodiment can be different from the order describing in detail in description in the above.Therefore, unless for example by such as " ... before ", " subsequently ", " in ... adjective special instruction afterwards " and so on, otherwise the sequence for the treatment of step in claim does not imply or needs the sequence of steps of permanent order.
For specific embodiment, advantage, other advantage and issue-resolution have been described above.But, advantage, advantage, issue-resolution, and can cause any advantage, advantage or solution appearance or the more significant any element (a plurality of) that becomes not to be interpreted as the key of any or whole claims, essential or essential characteristic or element.
Can to the present invention, make many modifications and variations according to instruction above, and these modifications and variations will be apparent to person of ordinary skill in the field.Scope of the present invention is defined by the following claims.
Claims (17)
1. a method, comprising:
Hollow high aspect ratio HAR sample is fixed in beam apparatus PBD, and wherein said hollow HAR sample has the tip of sealing; And
Described tip is contacted, until form perforate on described tip with the particle beams of described PBD; And
By the described hollow HAR sample characterization that forms described perforate on described tip, be wherein nanometer pipette.
2. basis the process of claim 1 wherein that the described tip of described hollow HAR sample has most advanced and sophisticated parameter and described contact has exposure parameter, and described method also comprises:
Select described PBD to become transmission electron microscope TEM, and use described TEM to described most advanced and sophisticated imaging;
Use described imaging to obtain described most advanced and sophisticated parameter; And
Use exposure parameter described in described most advanced and sophisticated parameter optimization.
3. according to the method for claim 2, wherein said hollow HAR sample is the nanometer test tube with wall thickness of being made by drawn glass, and described most advanced and sophisticated parameter comprises described wall thickness and point angle.
4. according to the method for claim 2, wherein said exposure parameter comprises particle beams intensity, particle beams diameter and the described duration contacting.
5. according to the method for claim 2, wherein said hole has the hole parameter that comprises desired value, and described method also comprises:
At described period of contact, use described imaging to obtain the described desired value of described hole parameter.
6. according to the method for claim 5, wherein said method also comprises:
If after described contact, described hole parameter is not described desired value, repeats described contact to obtain the described desired value of described hole parameter.
7. according to the process of claim 1 wherein that described method also comprises:
To promote the mode of the formation in described hole, select the environmental condition of described PBD inside.
8. according to the method for claim 7, wherein said environmental condition is included in 10
-3holder and 10
-7pressure between holder, and select precursor gases from oxygen-containing gas or hydrogen-containing gas or Halogen gas or their mixture.
9. a method, comprising:
The nanometer pipette with hole is fixed in beam apparatus (PBD), and wherein said hole has the hole parameter that comprises value and desired value; And
If described value is different from described desired value, make described nanometer pipette contact with the particle beams of described PBD, to obtain the described desired value of described hole parameter.
10. a system, comprising:
Hollow high aspect ratio HAR sample, it has the tip of sealing;
Beam apparatus PBD, it has the controlled particle beams and can fix described hollow HAR sample so that described tip is exposed to the mode of the described controlled particle beams;
The wherein said controlled particle beams can contact and form perforate in described tip with described tip; And
Wherein said system is characterized as being the setting for the manufacture of nanometer pipette.
11. according to the system of claim 10, wherein said PBD be can be to described most advanced and sophisticated imaging transmission electron microscope TEM, wherein said tip has the most advanced and sophisticated parameter that can obtain from described imaging, and wherein said contact has the exposure parameter that depends on described most advanced and sophisticated parameter.
12. according to the system of claim 11, and wherein said exposure parameter comprises particle beams intensity, particle beams diameter and the described duration contacting.
13. according to the system of claim 11, and wherein said hole has the hole parameter that comprises desired value, and can obtain described hole parameter from described imaging.
14. according to the system of claim 13, and wherein said hollow HAR sample is the nanometer test tube with wall thickness of being made by drawn glass, and described most advanced and sophisticated parameter comprises described wall thickness and point angle.
15. according to the system of claim 10, and the environmental condition of wherein said PBD inside is included in 10
-3holder and 10
-7pressure between holder, and select precursor gases from oxygen-containing gas or hydrogen-containing gas or Halogen gas or their mixture.
16. 1 kinds of systems, comprising:
The nanometer pipette with hole, wherein said hole has the hole parameter that comprises value and desired value, and wherein said value is different from described desired value;
Beam apparatus PBD, it has the controlled particle beams, and can be so that described nanometer pipette is exposed to the fixing described nanometer pipette of the mode of the described controlled particle beams; And
The wherein said controlled particle beams can contact with described nanometer pipette, and described value is become to described desired value.
17. 1 kinds of devices, comprising:
Hollow drawn glass main body, it has tapered end, and wherein said tapered end stops with hole, and surrounding's formation in wherein said hole is tubaeform; And
Wherein said device is characterized as being nanometer pipette.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US13/651,494 | 2012-10-15 | ||
| US13/651,494 US20140103582A1 (en) | 2012-10-15 | 2012-10-15 | Nano-Pipet Fabrication |
| US13/671,282 US20140105794A1 (en) | 2012-10-15 | 2012-11-07 | Nano-Pipet Fabrication |
| US13/671,282 | 2012-11-07 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103723672A true CN103723672A (en) | 2014-04-16 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310477529.8A Pending CN103723672A (en) | 2012-10-15 | 2013-10-14 | Device containing nano-pipet and fabrication method thereof |
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| US7041985B1 (en) * | 2004-11-12 | 2006-05-09 | Western Digital (Fremont), Inc. | Manipulator for microscopy sample preparation and methods for making and use thereof |
| US7173253B2 (en) * | 2003-01-31 | 2007-02-06 | Canon Kabushiki Kaisha | Object-moving method, object-moving apparatus, production process and produced apparatus |
| CN1942829A (en) * | 2004-06-07 | 2007-04-04 | 日本先锋公司 | Electron beam position fluctuation measurement method, electron beam position fluctuation measurement device, and electron beam recording device |
| CN1956787A (en) * | 2004-03-19 | 2007-05-02 | 埃斯珀·卡哈特 | Device for aspirating, manipulating, mixing and dispensing nano-volumes of liquids |
| US20080061249A1 (en) * | 2004-03-16 | 2008-03-13 | Board Of Regents, The University Of Texas System | High resolution low dose transmission electron microscopy real-time imaging and manipulation of nano-scale objects in the electron beam |
| US20090320624A1 (en) * | 2008-06-27 | 2009-12-31 | Omniprobe, Inc. | Method for Preparing Specimens for Atom Probe Analysis and Specimen Assemblies Made Thereby |
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2013
- 2013-10-14 CN CN201310477529.8A patent/CN103723672A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7173253B2 (en) * | 2003-01-31 | 2007-02-06 | Canon Kabushiki Kaisha | Object-moving method, object-moving apparatus, production process and produced apparatus |
| US20080061249A1 (en) * | 2004-03-16 | 2008-03-13 | Board Of Regents, The University Of Texas System | High resolution low dose transmission electron microscopy real-time imaging and manipulation of nano-scale objects in the electron beam |
| CN1956787A (en) * | 2004-03-19 | 2007-05-02 | 埃斯珀·卡哈特 | Device for aspirating, manipulating, mixing and dispensing nano-volumes of liquids |
| CN1942829A (en) * | 2004-06-07 | 2007-04-04 | 日本先锋公司 | Electron beam position fluctuation measurement method, electron beam position fluctuation measurement device, and electron beam recording device |
| US7041985B1 (en) * | 2004-11-12 | 2006-05-09 | Western Digital (Fremont), Inc. | Manipulator for microscopy sample preparation and methods for making and use thereof |
| US20090320624A1 (en) * | 2008-06-27 | 2009-12-31 | Omniprobe, Inc. | Method for Preparing Specimens for Atom Probe Analysis and Specimen Assemblies Made Thereby |
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Application publication date: 20140416 |