CN106290989B - A kind of atomic force microscope probe tip modification method - Google Patents
A kind of atomic force microscope probe tip modification method Download PDFInfo
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- CN106290989B CN106290989B CN201610587721.6A CN201610587721A CN106290989B CN 106290989 B CN106290989 B CN 106290989B CN 201610587721 A CN201610587721 A CN 201610587721A CN 106290989 B CN106290989 B CN 106290989B
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- 239000000523 sample Substances 0.000 title claims abstract description 89
- 238000002715 modification method Methods 0.000 title claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 230000018044 dehydration Effects 0.000 claims abstract description 9
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 235000019441 ethanol Nutrition 0.000 claims abstract description 7
- 239000005446 dissolved organic matter Substances 0.000 claims abstract description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 15
- 239000008103 glucose Substances 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 6
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000005034 decoration Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 17
- 238000012986 modification Methods 0.000 description 14
- 230000004048 modification Effects 0.000 description 13
- 239000000463 material Substances 0.000 description 5
- 229920002472 Starch Polymers 0.000 description 4
- 238000009395 breeding Methods 0.000 description 4
- 230000001488 breeding effect Effects 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000008107 starch Substances 0.000 description 4
- 235000019698 starch Nutrition 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910003481 amorphous carbon Inorganic materials 0.000 description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 description 3
- 239000002041 carbon nanotube Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 238000000418 atomic force spectrum Methods 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000005255 carburizing Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 150000002016 disaccharides Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000004621 scanning probe microscopy Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
- G01Q60/38—Probes, their manufacture, or their related instrumentation, e.g. holders
- G01Q60/42—Functionalisation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
- G01Q60/38—Probes, their manufacture, or their related instrumentation, e.g. holders
Abstract
The invention discloses a kind of atomic force microscope probe tip modification methods, this method is to stand 30min in the aqueous solution for immerse AFM probe dissolved organic matter, the AFM probe is further taken out to be dried, then the AFM probe after drying immerses in dehydration carburization agent, finally AFM probe is washed and dried to constant weight with ethyl alcohol to get the AFM probe needle point modified to carbon coating.This method has at low cost, simple operation and other advantages.
Description
Technical field
The invention belongs to the field of measuring technique of atomic force microscope, and in particular to a kind of atomic force microscope probe needle point
Method of modifying.
Background technique
As the technology of Material Field develops, probing into material surface microscopic appearance and microscopic characteristics becomes increasingly to weigh
It wants, the image of atomic resolution can be obtained by scanning probe microscopy.Atomic force microscope (AFM) is as scanning probe
Microscopical one kind, using between its probe tip atom and sample surfaces atom attraction and repulsive force obtain high-resolution
Rate image, AFM are not only a kind of tool of sample surfaces high-resolution imaging, can also be applied to obtain atomic force and distance
Relation curve, abbreviation force curve.It can provide the Local Property of material surface, such as elasticity, hardness, adhesion strength and surface charge
The valuable informations such as density.Core component of the AFM probe as atomic force microscope, acuity directly determine imaging
Lateral resolution, carbon nano-tube modified probe tip is a current research direction；And another developing direction is exactly probe
The functional modification of needle point, by that can measure various surface forces with qualitative, quantitative, be specific base in the specific substance of tip modification
The measurement of interaction force between group provides method, and can improve the clarity of characterization microscopic appearance.
The base material of average probe is Si3N4Or Si, at present there are mainly two types of the forms of probe tip modified carbon, carbon
Nanotube and diamond-like-carbon plated film, the purpose of both tip modifications are also different.Single can be prepared by CVD method
Pipe probe, the high transverse and longitudinal of carbon nanotube than structure, small radius of curvature, high Young's modulus can be improved atomic force microscope at
The lateral resolution of picture；Carpick(Carpick R W, Sridharan K, Sumant A V. DIAMOND-LIKE
CARBON COATED NANOPROBES:US, US20110107473 [P] 2011.) et al. pass through plasma chemistry gas
It is mutually deposited on the diamond like carbon layer that probe tip plates one layer of 5 ~ 60 nm thickness, to improve the wearability of needle point.Though these methods
Functional modification is so also achieved the purpose that, but it is high to operate equipment requirement, and needs professional operation, complex process.If only
It is then to need more easy method to modify probe to meet and be coated with the purpose of carbon in probe tip.
Summary of the invention
In view of the above shortcomings of the prior art, the purpose of the present invention is to provide a kind of at low cost, easy to operate
Atomic force microscope (AFM) probe tip method of modifying.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of atomic force microscope probe tip modification method, comprising the following steps:
1) aqueous solution of dissolved organic matter is prepared.
2) AFM probe is immersed in the aqueous solution that step 1) is prepared and stands 30min.During standing, this is conducive to can
The aqueous solution of soluble organism is sufficiently wet AFM probe, and dissolved organic matter is made fully to contact and be attached to AFM probe
Its surface.
3) AFM probe is taken out, dry 1 ~ 2h is placed under set environment, so that moisture evaporates, is allowed soluble organic
Object is deposited on AFM probe surface.
4) AFM probe after drying is immersed in dehydration carburization agent and stands 30min, make to be deposited on AFM probe surface can
Soluble organism carries out dehydration carburizing reagent, amorphous carbon is generated while removing H, O element, to realize carbon-coated purpose.
5) AFM probe is taken out, and is cleaned with ethyl alcohol to remove dehydration carburization agent, be subsequently placed under atmospheric environment and dry extremely
Constant weight is to get the AFM probe needle point modified to carbon coating.
Wherein, the aqueous solution for the dissolved organic matter that step 1) is prepared is that the glucose that mass fraction is 3 ~ 5wt% is water-soluble
Liquid.Since glucose is a kind of monosaccharide, molecular structure is relatively easy, property is stable, be more readily formed when dehydration carbonization
Relatively thin amorphous carbon layer.If, due to molecular structure complexity, dehydration carburizing reagent is not easy with this kind of disaccharide of sucrose or polysaccharide
Fully reacting, carbon-coated effect are undesirable.
And dehydration carburization agent described in step 4) is the concentrated sulfuric acid that mass fraction is 90 ~ 98wt%, this is mainly from cost
Consider, the concentrated sulfuric acid is more commonly to be dehydrated carburization agent, and property is stablized, and the noxious products after reaction are less.
In step 3), when the set environment is 60 DEG C of vacuum oven, drying time 1h；When the setting
Environment is atmosphere at room temperature environment, drying time 2h.
In order to accurately control the operating process of carbon coating modification, prevent AFM other parts from immersing in solution, the behaviour of step 2
As: AFM probe is fixed on syringe needle point, the AFM probe needle point is made to be in front end, syringe is clipped in contact
On angle tester, so that syringe is moved down into AFM probe needle point and submerge in the aqueous solution of step 1) preparation and stand 30min.
It is corresponding, the operation of step 3) are as follows: take out syringe, make the AFM probe needle point keep down, be placed in 60 DEG C
Dry 1h in vacuum oven.
The AFM probe is that substrate is Si3N4AFM probe.
Compared with prior art, the invention has the following beneficial effects:
The present invention has successfully coated one layer of very thin amorphous carbon using organic matter carbonizatin method in AFM probe needle point, is
The measurement of interaction force between special groups provides method, and the probe through organic matter carbonization modification carries out multiple AFM pattern
It can still be obtained after scanning and stablize clearly image, when doing force curve to specific sample surface, with the done power of unmodified probe
Curve generates difference to a certain degree.With it is existing by chemical vapor deposition method probe tip coated with carbon method phase
Than there is simple process, production cost is low, without large-scale precision instrument, simple operation and other advantages.
Detailed description of the invention
Fig. 1 is Si before modifying in embodiment 33N4AFM(atomic force microscope) probe tip SEM(electron-microscope scanning) figure；
Fig. 2 is Si after modifying in embodiment 33N4AFM probe needle point SEM figure；
Fig. 3 is using the Si before modification3N4AFM probe needle point scanning high starch breeding morphology characterization figure；
Fig. 4 is the Si after being modified using embodiment 33N4AFM probe needle point scanning high starch breeding morphology characterization figure.
Specific embodiment
Invention is further described in detail combined with specific embodiments below.
Embodiment 1
Carbon coating modification is carried out to atomic force microscope (AFM) probe tip using following steps:
(1) it weighs 0.05g glucose to be dissolved in 0.95mL deionized water, is stirred to dissolve, be prepared with glass bar
The glucose solution of mass fraction 5wt%；
It (2) is Si by substrate3N4AFM(atomic force microscope) probe is directly immersed in the glucose solution in (1), quiet
30min is set, is taken out；
(3) by 1h dry under the conditions of the probe of taking-up in a vacuum drying oven 60 DEG C；
(4) probe after drying is immersed mass fraction is to stand 30min in 90 ~ 98wt% concentrated sulfuric acid；
(5) naturally dry after probe is cleaned with a small amount of ethyl alcohol is taken out.
Embodiment 2
Carbon coating modification is carried out to atomic force microscope (AFM) probe tip using following steps:
(1) it weighs 0.05g glucose to be dissolved in 0.95mL deionized water, is stirred to dissolve, be prepared with glass bar
The glucose solution of mass fraction 5wt%；
It (2) is Si by substrate3N4AFM probe be directly immersed in the glucose solution in (1), stand 30min；
(3) naturally dry 2h after taking out；
(4) it is to stand 30min in 90 ~ 98wt% concentrated sulfuric acid that the probe after drying, which immerses mass fraction,；
(5) naturally dry after probe is cleaned with a small amount of ethyl alcohol is taken out.
Embodiment 3
Carbon coating modification is carried out to atomic force microscope (AFM) probe tip using following steps:
(1) it weighs 0.05g glucose to be dissolved in 0.95mL deionized water, is stirred to dissolve, be prepared with glass bar
The glucose solution of mass fraction 5wt%；
It (2) is Si by substrate3N4AFM probe (its SEM figure is shown in Fig. 1) be fixed to syringe needle point on, probe tip is in
Syringe is clipped in contact angle tester by front end, and by observing monitor, syringe is slowly moved down into probe tip
Stop in the glucose solution just submerged in (1), stands 30min；
(3) syringe is taken out the cone of probe tip keeps down and dries under the conditions of 60 DEG C in a vacuum drying oven
1h；；
(4) probe after drying is immersed mass fraction is to stand 30min in 90 ~ 98wt% concentrated sulfuric acid；
(5) naturally dry after probe is cleaned with a small amount of ethyl alcohol is taken out, the AFM probe needle point of carbon coating modification, SEM are obtained
Figure is shown in Fig. 2.
Embodiment 4
Carbon coating modification is carried out to atomic force microscope (AFM) probe tip using following steps:
(1) it weighs 0.03g glucose to be dissolved in 0.97mL deionized water, is stirred to dissolve, be prepared with glass bar
The glucose solution of mass fraction 3wt%；
It (2) is Si by substrate3N4AFM probe be directly immersed in the glucose solution in (1), stand 30min, take out；
(3) by 1h dry under the conditions of the probe of taking-up in a vacuum drying oven 60 DEG C；
(4) probe after drying is immersed mass fraction is to stand 30min in 90 ~ 98wt% concentrated sulfuric acid；
(5) naturally dry after probe is cleaned with a small amount of ethyl alcohol is taken out.
Embodiment 5
Using unmodified Si3N4The Si of needle point and the method modified of embodiment 33N4Needle point is respectively to high starch breeding
Be scanned to obtain morphology characterization figure, shown in respectively Fig. 3 and Fig. 4, by comparison it can be found that Fig. 3 it is whole more it is smooth
It is even, and Fig. 4 shows that color has certain variation, that is, shows the variation of active force.It can be found that by modification and it is unmodified
Probe has difference when measuring high starch breeding surface topography, carries out surface sweeping with the probe after modification, can obtain more
Minutia.After modified, surface topography depth degree can also change, it was demonstrated that there are active force variations, but substantially special
Sign will not change, it ensure that the integrality of measurement.
It is possible thereby to prove, the Si of modified3N4Needle point ensure that original Si3N4It, can be on the basis of the function of needle point
New performance is obtained, this is of great significance to for the research of material surface property.
The above embodiment of the present invention is only example to illustrate the invention, and is not to implementation of the invention
The restriction of mode.For those of ordinary skill in the art, other can also be made not on the basis of the above description
With the variation and variation of form.Here all embodiments can not be exhaustive.It is all to belong to technical solution of the present invention
Changes and variations that derived from are still in the scope of protection of the present invention.
Claims (6)
1. a kind of atomic force microscope probe tip modification method, which comprises the following steps:
1) aqueous solution of dissolved organic matter is prepared；The aqueous solution of the dissolved organic matter is that mass fraction is 3 ~ 5wt%
Glucose solution；
2) AFM probe is immersed in the aqueous solution that step 1) is prepared and stands 30min；
3) AFM probe is taken out, dry 1 ~ 2h is placed under set environment；
4) AFM probe after drying is immersed in dehydration carburization agent and stands 30min；The dehydration carburization agent is that mass fraction is
The concentrated sulfuric acid of 90 ~ 98wt%；
5) AFM probe is taken out, and is cleaned with ethyl alcohol, be subsequently placed in drying under atmospheric environment and repaired to constant weight to get to carbon coating
The AFM probe needle point of decorations.
2. atomic force microscope probe tip modification method according to claim 1, which is characterized in that described in step 3)
Set environment be 60 DEG C of vacuum oven, drying time 1h.
3. atomic force microscope probe tip modification method according to claim 1, which is characterized in that described in step 3)
Set environment be atmosphere at room temperature environment, drying time 2h.
4. atomic force microscope probe tip modification method according to claim 1, which is characterized in that the operation of step 2
Are as follows: AFM probe is fixed on syringe needle point, so that the AFM probe needle point is in front end, syringe is clipped in contact angle
On tester, so that syringe is moved down into AFM probe needle point and submerge in the aqueous solution of step 1) preparation and stand 30min.
5. atomic force microscope probe tip modification method according to claim 1, which is characterized in that the operation of step 3)
Are as follows: syringe is taken out, the AFM probe needle point is made to keep down, is placed in 60 DEG C of vacuum oven dry 1h.
6. -5 any atomic force microscope probe tip modification method according to claim 1, which is characterized in that described
AFM probe is that substrate is Si3N4AFM probe.
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| CN107043929B (en) * | 2017-03-23 | 2019-08-16 | 中国科学院化学研究所 | A method of the coat of metal is generated in atomic force microscope probe surface zone of control |
| CN107015029B (en) * | 2017-05-11 | 2019-12-13 | 四川理工学院 | Method for making carbon material sample for atomic force microscope contact mode characterization |
| CN108398578B (en) * | 2018-01-15 | 2019-12-17 | 大连理工大学 | Method for modifying atomic force microscope probe by using magnetic nanoparticles |
| CN108375687B (en) * | 2018-03-09 | 2020-12-04 | 北京协同创新研究院 | Method for coating graphene on probe tip of atomic force microscope |
| CN109470891A (en) * | 2018-11-08 | 2019-03-15 | 国网山东省电力公司电力科学研究院 | A kind of probe modification method of atomic force microscope |
| CN113219211B (en) * | 2021-04-28 | 2022-02-22 | 西安交通大学 | Preparation method of nano probe |
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| JP2624873B2 (en) * | 1990-05-16 | 1997-06-25 | 松下電器産業株式会社 | Atomic force microscope probe and method of manufacturing the same |
| JP3123497B2 (en) * | 1998-03-02 | 2001-01-09 | 日本電気株式会社 | Evaluation method of orientation of liquid crystal alignment film by atomic force microscope |
| CN1790799A (en) * | 2004-12-14 | 2006-06-21 | 中国电子科技集团公司第十八研究所 | High power lithium ion battery and method for preparing amorphous carbon coated anode material |
| CN1815181A (en) * | 2005-02-02 | 2006-08-09 | 北京大学 | Single-wall carbon nano-tube point and preparing method |
| CN100573733C (en) * | 2006-03-03 | 2009-12-23 | 北京大学 | Field optical fibre probe and preparation method thereof |
| CN101696980A (en) * | 2009-10-27 | 2010-04-21 | 北京大学 | Method for preparing pinpoint of nano-tungsten probe |
| CN102633300A (en) * | 2011-12-07 | 2012-08-15 | 天津市贝特瑞新能源材料有限责任公司 | Carbon-coated lithium titanate cathode material as well as preparation method and applications thereof |
| CN102969492B (en) * | 2012-12-04 | 2014-11-12 | 广州有色金属研究院 | Carbon-coated doping modified lithium titanate and preparation method thereof |
| CN104360107B (en) * | 2014-11-12 | 2016-11-30 | 苏州大学 | A kind of graphene coated atomic force microscope probe and preparation method thereof, purposes |
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