CN103389392A - Preparation method for nano-probe capable of measuring AFM mechanical parameter - Google Patents
Preparation method for nano-probe capable of measuring AFM mechanical parameter Download PDFInfo
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- CN103389392A CN103389392A CN2013103151776A CN201310315177A CN103389392A CN 103389392 A CN103389392 A CN 103389392A CN 2013103151776 A CN2013103151776 A CN 2013103151776A CN 201310315177 A CN201310315177 A CN 201310315177A CN 103389392 A CN103389392 A CN 103389392A
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Abstract
The invention provides a preparation method for a nano-probe capable of measuring an AFM mechanical parameter. Products required by the preparation of the nano-probe comprise a tipless micro-cantilever probe, a micro-ball with the diameter of 2-5 Mum or 5-10 Mum, ethylene oxide resin adhesive, a dedicated mixing cutter, a standard glass slide with accurate scales or an SEM, a biological type AFM with an optical microscope and an imaging system, wherein the nano-probe of the micro-cantilever is used in combination with the biological type AFM. According to the method, steps of replacing the needle tip, calibrating laser, and replacing of a pin with the micro-ball for the measuring of the mechanical parameter are not required after each time of imaging, and as a result, the operation is simple, and the measured mechanical parameter is more accurate.
Description
Technical field
The present invention relates to a kind of nano-probe preparation method of the AFM of measurement mechanics parameter, belong to field of mechanical technique.
Background technology
The application of nanometer technology has brought huge development prospect to medical science, life science, pharmacy, chemistry and biological detection, manufacturing industry, optics and national defence etc. field.Use the nanometer technique means to solve the problem that a lot of classical theories cannot be considered.And AFM is as one of key instrument of studying micro-nano-scale, in recent years, the recoverable amount of the large-scale research institution such as research institute and colleges and universities constantly increases at home, but meanwhile, the consumption of the expensive easy consumption material that matches with it---nano-probe is rapid growth also.But, according to traditional AFM design concept, to pursue high-resolution imaging in using probe scanning, just be difficult to obtain simultaneously accurate mechanical property parameter measurement.
Summary of the invention
the invention provides a kind of nano-probe preparation method of the AFM of measurement mechanics parameter, can overcome the above defect of telling, lead to traditional taper or pyramid needle point are modified, use microballoon to modify and not only can meet high-resolution pattern parsing but also can realize that mechanics parameter is measured accurately, avoid the damage problem due to the huge pressure cell membrane of needle point single-point, meet common laboratory cost degradation principles and requirements, a kind of practicality is provided, low-cost, function admirable, can obtain accurate mechanics parameter and measure ground, the synchronism consistance is nano-probe microballoon modification preparation method preferably, to meet society and the market demand.Thereby the mechanics parameter that is used for Measurement accuracy normal cell and the nano-scale degree such as cancer cell, tissue, material and surface particles thing, for micro-nano research field provides a kind of reliable means.
For solving above technical matters, the invention provides following technical scheme: a kind of nano-probe preparation method of the AFM of measurement mechanics parameter, it is characterized in that, prepare the nano-probe required product and comprise: micro-cantilever tipless cantilever, diameter be 2-5um or 5um-10um microballoon, ethylene oxide resin glue, special-purpose transfer mix cutter, with the standard microslide of exact scale or SEM, bion AFM with optical microscope and imaging system; The nano-probe of described micro-cantilever and bion AFM coupling; SEM is that scanning electron microscope, bion AFM are atomic force microscope, and the step of described probe preparation method is as follows:
A. the micro-cantilever probe is inserted AFM, by normal operation step, set up and the laser focusing hot spot, it is aligned in the soon zone of cementation microballoon.
B. after setting up laser and focusing, after making the suitable Sum value of acquisition, make laser facula focus to the four-quadrant center, withdraw stepper motor and syringe needle, place the microballoon on microslide and microslide.
C. microballoon is layered in advance in a territory, lateral areas of clean microslide, and takes off the AFM scanner head, place and to be the microslide that microballoon is arranged and to put the AFM sample stage and fix, and utilize form, size and the uniformity coefficient of CCD observation post paving microballoon.
D. properly placement is standby to take off the microballoon microslide from AFM, and microslide, at the AFM microscopically, is implemented microoperation promotion microballoon with the AFM micro-cantilever and moved among a small circle the demarcation zone of standard film, thereby determine the size diameter of institute's micrometer ball, after complete operation, change the microballoon of known dimensions, standby.
E. be covered with the microslide of the microballoon of known dimensions specification before relaying, put the AFM sample stage and fix, beamhouse operation.
F. advance the AFM stepper motor to the microsphere surface near on slide, careful observation and select the microballoon in the microoperation zone of wanting again under CCD that AFM carries is auxiliary, and with little marker pen as little mark, certain zone is elected to be operational zone.
G. remove stepper motor, lift pin, take off microslide, properly place standby; Separately get a clean microslide and be used for the mediation epoxide-resin glue, after two kinds of paste compositions of epoxy resin are pressed the mixing of 1:1 equal-volume, transfer and mix evenly rapidly.
H. get before recorded size specification microballoon a little, be placed in the opposite side of clean slide, standby.
I. fixing microslide, CD-ROM drive motor advances stepper motor, lower pin.
G. open CD-ROM drive motor and advance stepper motor, prepare to dip in glue in micro-cantilever.
K. after playing pin to micro-cantilever gently to contact glue, after slightly dipping in a little glue, do not lift pin and drag round about micro-cantilever and erase unnecessary glue.
L. then lift pin, hand adjustment AFM sample stage moves to the microballoon zone that performs mark, position is just in time set up in micro-cantilever tip location center, lower pin, until touch microballoon above, stagnate 30s-1min.
M. lift needle point and microballoon on, withdraw upward 50um to stepper motor, braking, wait for that epoxy resin solidifies fully.
Further, described nano-probe micro-cantilever is shaped as rectangle, flechette-type, V-arrangement or triangle.
Further, described microballoon is monodisperse system polystyrene microsphere, glass microsphere or SiO
2Microballoon.
The nano-probe preparation method of this AFM of the measurement mechanics parameter that the present invention relates to, the beneficial effect that has:
1. self assembling type micro-cantilever nano-probe and microballoon can reduce the cost in laboratory.
2. the microballoon of the above monodisperse system of 2-5um and 5um can be taken into account high-resolution imaging and mechanics parameter is measured, and need not each imaging and change needle point, calibration laser after complete, more more the pin of tape swapping microballoon goes the step of ergometry mathematic(al) parameter.
3. ethylene oxide resin glue can provide sufficiently solid bonding force for probe cantilever and microballoon, and can guarantee its set time to complete smoothly in the microoperation that microscopically is implemented.
4. use the diameter that is used for determining the monodisperse system microballoon with the standard film of exact scale and SEM, simple and easy to do, degree of accuracy is high.
5. the AFM microscopic system can provide a kind of micro-nano-scale feasible method for enforcement microoperation or little modification in visible visual field.
6. can avoid the huge pressure of needle point single-point to biomembranous damage and self the intrinsic needle point deviation problem that makes progress without the decline combination of cantilever probe and minimicrosphere of needle point, make the mechanics parameter of measurement more accurate.
Description of drawings
Fig. 1 is nano-probe structural representation of the present invention;
Fig. 2 is that nanometer of the present invention is visited knot pin structure schematic diagram;
Fig. 3 is nano-probe structural representation of the present invention;
Fig. 4 monodisperse system polystyrene microsphere of the present invention, glass bead or SiO
2The micro-sphere structure schematic diagram;
Fig. 5 the present invention transfers and mixes the knife structure schematic diagram;
Fig. 6 and Fig. 7 are microslide of the present invention and preparation process schematic diagram;
Fig. 8 and Fig. 9 are nano-probe of the present invention and micro-sphere structure figure;
Figure 10 is the probe clamp structural drawing of bion AFM optical microphotograph imaging system.
Embodiment
As shown in Figure 1-Figure 3, micro-cantilever is respectively rectangle, flechette-type and triangle.
This preparation method can be used for various normal cells and the mechanical property of the nano-scale degree such as cancer cell, tissue, material and surface particles thing and the Measurement accuracy of parameter, especially for the object of nano-scale, measures and imaging.Equipment and instrument that the preparation method comprises are as follows: the nano-probe of micro-cantilever, micro-cantilever be within 2um-5um and more than 5um, the polystyrene microsphere of monodisperse system, glass microsphere, perhaps SiO
2Microballoon, ethylene oxide resin glue and special-purpose the accent are mixed cutter, and with standard microslide (25*75* thickness 3mm, transparent) or the SEM of exact scale, bion AFM is with optical microscope and imaging system.As shown in Figure 4 and Figure 5, mix knife structure figure for microballoon and accent.
As shown in Fig. 6-10, be the preparation process schematic diagram.The described nano-probe 1 of this method and bion AFM coupling, the described microslide of standard with exact scale 5 and SEM are for determining the diameter of monodisperse system microballoon 2, and ethylene oxide resin glue 3 and special-purpose the accent are mixed cutter for cementation microballoon 2.its concrete grammar is: at first nano-probe 1 is arranged on the AFM scanner head, the micro-cantilever 11 of nano-probe 1, carry out the AFM calibration, then lift the microscope condenser, take off scanner head, monodisperse system microballoon 2 is decanted some to microslide 5, then, the microslide 5 that is loaded with microballoon is put back to AFM sample fixed station to be fixed, again put back focus lamp, set pin under initial value, progressively approach under the driving of stepper motor, after reaching microslide 5 surfaces, lift pin 200um, that probe 1 leaves microslide 5 surfaces, focusing on microballoon 2, observe size and the uniformity coefficient of microballoon 2, choose want the zone of bonding microballoon 2, and with the Marker pen, do little mark, probe 1 is thoroughly being left surface of glass slide, take off at the slide that microballoon 2 is arranged standby, separately go the clean microslide of a slice 5 to be used for mediation epoxide-resin glue 3, respectively get pulvis and liquor 1:1(v/v), transfer and mix the cutter mediation with plastics, be 5-10min the set time of general this kind epoxide-resin glue 3, after being in harmonious proportion evenly, get a little glue, put with the zone that microballoon 2 is arranged near, fix this year of 5 of glass, under the adjusting condenser, pin is to the edge of resin glue, find position, play gently pin to after contacting glue, withdraw rapidly the surface of glue, look under a white space pin to contacting microslide 5 bottoms, this moment, careful motion scan pin was erased unnecessary glue, with regulating sample stage, be afterwards the below that the microballoon zone of marking in advance mark is pin, advance stepper motor to make pin approach the microballoon aspect, again determine the microballoon 2 that will operate, lower pin is to microballoon 2, perhaps play pin to the white space nearer apart from microballoon, after lifting pin 100, microballoon 2 is moved under pin, probe 1 is contacted with microballoon 2, various AFM all has demonstration (such as JPK is idle), keep this state to stagnate several seconds, then remove pin 100um, any vibrations do not appear, wait for that the 30min left and right is thoroughly solidified glue, so far complete all processes that the probe microballoon is modified.
the nano-probe preparation method of this AFM of the measurement mechanics parameter that present technique provides, can meet high-resolution pattern for traditional taper or pyramid needle point and resolve and can not realize that mechanics parameter is measured accurately, be prone to the damage problem of the huge pressure of single-point of needle point for cell membrane, and the application specific probe cost of the load microballoon after improving is too high, can not meet the requirement of common laboratory cost degradation principle, therefore this method makes up above-mentioned main deficiency, proposed practicably a kind of, low-cost, can obtain accurate mechanics parameter and measure ground, the synchronism consistance is nano-probe microballoon method of modifying preferably, be used for Measurement accuracy normal cell and cancer cell, tissue, the mechanics parameter of the nano-scale degree such as material and surface particles thing, for micro-nano research field provides a kind of reliable means.
Embodiment of the present invention does not form the restriction to the application's scope; every within the spirit and principle of the present invention design, any modification that one of skill in the art can make, be equal to and replace and within improvement etc. all should be included in protection scope of the present invention.
Claims (3)
1. nano-probe preparation method that can measure the AFM mechanics parameter, it is characterized in that, prepare the nano-probe required product and comprise: micro-cantilever probe, diameter be 2-5um microballoon, ethylene oxide resin glue, special-purpose transfer mix cutter, with the standard microslide of exact scale or SEM, bion AFM with optical microscope and imaging system; The nano-probe of described micro-cantilever and bion AFM coupling; The step of described probe preparation method is as follows:
The micro-cantilever probe is inserted AFM, by normal operation step, set up and the laser focusing hot spot, it is aligned in the soon zone of cementation microballoon;
After setting up laser and focusing, after making the suitable Sum of acquisition, make laser facula focus to the four-quadrant center, withdraw stepper motor and syringe needle, place the microballoon on microslide and microslide;
Microballoon is layered in advance in a territory, lateral areas of clean microslide, and takes off the AFM scanner head, place and to be the microslide that microballoon is arranged and to put the AFM sample stage and fix, and utilize the form of CCD observation post paving microballoon, size and uniformity coefficient;
D. properly placement is standby to take off the microballoon microslide from AFM, and microslide, at the AFM microscopically, is implemented microoperation promotion microballoon with the AFM micro-cantilever and moved among a small circle the demarcation zone of standard film, thereby determine the size diameter of institute's micrometer ball, after complete operation, change the microballoon of known dimensions, standby;
E. be covered with the microslide of the microballoon of known dimensions specification before relaying, put the AFM sample stage and fix, beamhouse operation;
F. advance the AFM stepper motor to the microsphere surface near on slide, careful observation and select the microballoon in the microoperation zone of wanting again under CCD that AFM carries is auxiliary, and with little marker pen as little mark, certain zone is elected to be operational zone;
G. remove stepper motor, lift pin, take off microslide, properly place standby; Separately get a clean microslide and be used for the mediation epoxide-resin glue, after two kinds of paste compositions of epoxy resin are pressed the mixing of 1:1 equal-volume, transfer rapidly and mix evenly;
H. get before recorded size specification microballoon a little, be placed in the opposite side of clean slide, standby;
I. fixing microslide, CD-ROM drive motor advances stepper motor, lower pin;
G. open CD-ROM drive motor and advance stepper motor, prepare to dip in glue in micro-cantilever;
K. after playing pin to micro-cantilever gently to contact glue, after slightly dipping in a little glue, do not lift pin and drag round about micro-cantilever and erase unnecessary glue;
L. then lift pin, hand adjustment AFM sample stage moves to the microballoon zone that performs mark, position is just in time set up in micro-cantilever tip location center, lower pin, until touch microballoon above, stagnate 30s-1min;
M. lift needle point and microballoon on, withdraw upward 50um to stepper motor, braking, wait for that epoxy resin solidifies fully.
2. a kind of nano-probe preparation method who measures the AFM mechanics parameter according to claim 1, is characterized in that, described nano-probe micro-cantilever be shaped as rectangle, flechette-type, V-arrangement or triangle.
3. a kind of nano-probe preparation method who measures the AFM mechanics parameter according to claim 1, is characterized in that, described microballoon is monodisperse system polystyrene microsphere, glass microsphere or SiO
2Microballoon.
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Cited By (9)
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| WO2016107534A1 (en) * | 2014-12-29 | 2016-07-07 | 史拓莱姆有限公司 | Detection device having attached probe |
| CN107796958A (en) * | 2017-09-18 | 2018-03-13 | 上海理工大学 | A kind of preparation method of AFM colloid probe |
| CN108369220A (en) * | 2015-10-22 | 2018-08-03 | 巴塞尔大学 | The nanometer mechanics of breast cancer molecular subtypes are analyzed |
| CN109444476A (en) * | 2018-10-15 | 2019-03-08 | 上海交通大学 | A kind of preparation method of atomic force microscope sub-micron probe |
| CN109521227A (en) * | 2018-10-21 | 2019-03-26 | 天津大学 | A kind of fast preparation method and application of colloid probe |
| CN110057751A (en) * | 2018-01-19 | 2019-07-26 | 清华大学 | The making apparatus and method of optical particle probe |
| CN110155938A (en) * | 2019-06-11 | 2019-08-23 | 西南交通大学 | A kind of microsphere probe preparation method based on micro-cantilever transfer |
| CN111505346A (en) * | 2020-05-15 | 2020-08-07 | 大连理工大学 | AFM probe for quantitative measurement, modification method and application thereof |
| CN113267649A (en) * | 2021-04-29 | 2021-08-17 | 大连海事大学 | Preparation method of long-arm probe of atomic force microscope |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016107534A1 (en) * | 2014-12-29 | 2016-07-07 | 史拓莱姆有限公司 | Detection device having attached probe |
| CN106716142A (en) * | 2014-12-29 | 2017-05-24 | 史拓莱姆有限公司 | Detection device having attached probe |
| CN108369220A (en) * | 2015-10-22 | 2018-08-03 | 巴塞尔大学 | The nanometer mechanics of breast cancer molecular subtypes are analyzed |
| US11686720B2 (en) | 2015-10-22 | 2023-06-27 | Universitat Basel | Nanomechanical profiling of breast cancer molecular subtypes |
| CN107796958A (en) * | 2017-09-18 | 2018-03-13 | 上海理工大学 | A kind of preparation method of AFM colloid probe |
| CN110057751A (en) * | 2018-01-19 | 2019-07-26 | 清华大学 | The making apparatus and method of optical particle probe |
| CN110057751B (en) * | 2018-01-19 | 2021-06-29 | 清华大学 | Apparatus and method for fabricating optical particle probe |
| CN109444476A (en) * | 2018-10-15 | 2019-03-08 | 上海交通大学 | A kind of preparation method of atomic force microscope sub-micron probe |
| CN109521227A (en) * | 2018-10-21 | 2019-03-26 | 天津大学 | A kind of fast preparation method and application of colloid probe |
| CN110155938A (en) * | 2019-06-11 | 2019-08-23 | 西南交通大学 | A kind of microsphere probe preparation method based on micro-cantilever transfer |
| CN110155938B (en) * | 2019-06-11 | 2022-01-28 | 西南交通大学 | Method for preparing microsphere probe based on micro-cantilever transfer |
| CN111505346A (en) * | 2020-05-15 | 2020-08-07 | 大连理工大学 | AFM probe for quantitative measurement, modification method and application thereof |
| CN113267649A (en) * | 2021-04-29 | 2021-08-17 | 大连海事大学 | Preparation method of long-arm probe of atomic force microscope |
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