CN106290989A - 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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- CN106290989A CN106290989A CN201610587721.6A CN201610587721A CN106290989A CN 106290989 A CN106290989 A CN 106290989A CN 201610587721 A CN201610587721 A CN 201610587721A CN 106290989 A CN106290989 A CN 106290989A
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- force microscope
- afm probe
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- 239000000523 sample Substances 0.000 title claims abstract description 91
- 238000002715 modification method Methods 0.000 title claims abstract description 12
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 238000005034 decoration Methods 0.000 claims abstract description 9
- 230000018044 dehydration Effects 0.000 claims abstract description 8
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 238000010926 purge Methods 0.000 claims abstract description 7
- 239000005446 dissolved organic matter Substances 0.000 claims abstract description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 235000011149 sulphuric acid Nutrition 0.000 claims description 7
- 239000001117 sulphuric acid Substances 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000005253 cladding Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 16
- 239000011248 coating agent Substances 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 abstract description 8
- 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 description 14
- 239000008103 glucose Substances 0.000 description 14
- 239000000243 solution Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 6
- 230000008859 change Effects 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
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000008107 starch Substances 0.000 description 4
- 235000019698 starch Nutrition 0.000 description 4
- 238000003756 stirring Methods 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
- 238000000418 atomic force spectrum Methods 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000012876 topography Methods 0.000 description 3
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000005255 carburizing Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 108010001394 Disaccharidases Proteins 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
- 229930006000 Sucrose Natural products 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 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
- 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 method, the method is standing 30min in the aqueous solution that AFM probe immerses dissolved organic matter, further take out described AFM probe to be dried, the most dried AFM probe immerses in dehydration carburization agent, finally by AFM probe ethanol purge and be dried to constant weight, i.e. obtain the AFM probe needle point of carbon coating decoration.This method has low cost, simple operation and other advantages.
Description
Technical field
The invention belongs to the field of measuring technique of atomic force microscope, be specifically related to a kind of atomic force microscope probe needle point
Method of modifying.
Background technology
Along with the technology of Material Field develops, probe into material surface microscopic appearance and microscopic characteristics becomes increasingly to weigh
Want, the image of atomic resolution can be obtained by scanning probe microscopy.Atomic force microscope (AFM) is as scanning probe
Microscopical one, utilizes the captivation between its probe tip atom and sample surfaces atom and repulsive force to obtain high-resolution
Rate image, AFM is not only a kind of instrument of sample surfaces high-resolution imaging, it is also possible to be applied to obtain atomic force and distance
Relation curve, be called for short force curve.It is provided that the Local Property of material surface, such as elasticity, hardness, adhesion and surface charge
The valuable information such as density.AFM probe is as the core component of atomic force microscope, and its acuity directly determines imaging
Lateral resolution, probe tip is carbon nano-tube modified is a current research direction；And another developing direction is exactly probe
The functional modification of needle point, by the specific material of tip modification, can measure various surface forces with qualitative, quantitative, for specific base
The measurement of the interaction force between group provides method, it is possible to improve the definition characterizing microscopic appearance.
The base material of average probe is Si3N4Or Si, the form at probe tip modified carbon mainly has two kinds at present, carbon
Nanotube and diamond-like-carbon plated film, the purpose of both tip modifications is the most different.Single can be prepared by CVD
Pipe probe, the high transverse and longitudinal of CNT can improve atomic force microscope than structure, little radius of curvature, high Young's modulus
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. by plasma chemistry gas
It is deposited on probe tip mutually and plates one layer of 5 ~ 60 diamond like carbon layer thick for nm, in order to improve the wearability of needle point.Though these methods
So also reach the purpose of functional modification, but operation equipment requirements is high, and need professional operation, complex process.If only
It is to meet the purpose being coated with carbon at probe tip, then needs the easiest method that probe is modified.
Summary of the invention
For deficiencies of the prior art, it is an object of the invention to provide a kind of low cost, simple to operate
Atomic force microscope (AFM) probe tip method of modifying.
To achieve these goals, the technical solution used in the present invention is as follows:
A kind of atomic force microscope probe tip modification method, comprises the following steps:
1) aqueous solution of dissolved organic matter is prepared.
2) AFM probe is immersed and the aqueous solution of step 1) preparation stands 30min.During standing, this beneficially may be used
The aqueous solution of soluble organism is sufficiently wet AFM probe, makes dissolved organic matter contact with AFM probe fully and be attached to
Its surface.
3) AFM probe described in taking-up, is placed under set environment and is dried 1 ~ 2h, so that moisture evaporation, makes solubility organic
Thing is deposited on AFM probe surface.
4) being immersed in dehydration carburization agent by dried AFM probe and stand 30min, make to be deposited on AFM probe surface can
Soluble organism carries out being dehydrated carburizing reagent, generates amorphous carbon while removing H, O element, to realize the purpose of carbon cladding.
5) AFM probe is taken out, and removes dehydration carburization agent with ethanol purge, be subsequently placed under atmospheric environment be dried to
Constant weight, i.e. obtains the AFM probe needle point of carbon coating decoration.
Wherein, the aqueous solution of dissolved organic matter of step 1) preparation be mass fraction be that the glucose of 3 ~ 5wt% is water-soluble
Liquid.Owing to glucose is a kind of monosaccharide, its molecular structure is relatively easy, stable in properties, carries out being more readily formed when being dehydrated carbonization
Relatively thin amorphous carbon layer.If with this kind of disaccharidase of sucrose or polysaccharide, owing to molecular structure is complicated, dehydration carburizing reagent is difficult to
Completely, the effect of carbon cladding is undesirable in reaction.
And the dehydration carburization agent described in step 4) be mass fraction is the concentrated sulphuric acid of 90 ~ 98wt%, this is mainly from cost
Considering, concentrated sulphuric acid is the dehydration carburization agent more commonly used, and stable in properties, reacted noxious products is less.
In step 3), when the vacuum drying oven that described set environment is 60 DEG C, drying time is 1h；When described setting
Environment is atmosphere at room temperature environment, and drying time is 2h.
In order to accurately control the operating process of carbon coating decoration, other are partly submerged in solution to prevent AFM, step 2) behaviour
As: AFM probe is fixed on syringe needle point, makes described AFM probe needle point be in foremost, syringe is clipped in contact
On angle tester, make syringe be moved down into AFM probe needle point submerge step 1) preparation aqueous solution in and stand 30min.
Corresponding, the operation of step 3) is: takes out syringe, makes described AFM probe needle point keep down, be placed in 60 DEG C
Vacuum drying oven is dried 1h.
Described AFM probe be substrate be Si3N4AFM probe.
Compared with prior art, there is advantages that
The present invention uses organic carbonizatin method to be successfully coated with the thinnest one layer amorphous carbon at AFM probe needle point, for specific
The measurement of the interaction force between group provides method, and the probe modified through organic carbonization carries out repeatedly AFM topography scan
After be still obtained in that stable image the most clearly, when force curve is done on specific sample surface, force curve done with unmodified probe
Produce to a certain degree difference.With existing by chemical vapor deposition method in the method for probe tip coated with carbon compared with, tool
Having technique simple, production cost is low, it is not necessary to by large-scale precision instrument, simple operation and other advantages.
Accompanying drawing explanation
Fig. 1 is to modify front Si in embodiment 33N4AFM(atomic force microscope) the SEM(electron-microscope scanning of probe tip) figure；
Fig. 2 be in embodiment 3 modify after Si3N4AFM probe needle point SEM figure；
Fig. 3 is to use the Si before modifying3N4The morphology characterization figure of AFM probe needle point scanning high starch breeding；
Fig. 4 is the Si after using embodiment 3 to modify3N4The morphology characterization figure of AFM probe needle point scanning high starch breeding.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
Use following steps that atomic force microscope (AFM) probe tip carries out carbon coating decoration:
(1) weigh 0.05g glucose to be dissolved in 0.95mL deionized water, make it dissolve with Glass rod stirring, prepare quality
The glucose solution of mark 5wt%；
(2) it is Si by substrate3N4AFM(atomic force microscope) probe is directly immersed in the glucose solution in (1), stand
30min, takes out；
(3) probe taken out is dried in vacuum drying oven 1h under the conditions of 60 DEG C；
(4) dried probe immersing mass fraction is standing 30min in 90 ~ 98wt% concentrated sulphuric acid；
(5) take out probe naturally to dry after a small amount of ethanol purge.
Embodiment 2
Use following steps that atomic force microscope (AFM) probe tip carries out carbon coating decoration:
(1) weigh 0.05g glucose to be dissolved in 0.95mL deionized water, make it dissolve with Glass rod stirring, prepare quality
The glucose solution of mark 5wt%；
(2) it is Si by substrate3N4AFM probe be directly immersed in the glucose solution in (1), stand 30min；
(3) 2h is naturally dried after taking out；
(4) it is standing 30min in 90 ~ 98wt% concentrated sulphuric acid that the probe after drying immerses mass fraction；
(5) take out probe naturally to dry after a small amount of ethanol purge.
Embodiment 3
Use following steps that atomic force microscope (AFM) probe tip carries out carbon coating decoration:
(1) weigh 0.05g glucose to be dissolved in 0.95mL deionized water, make it dissolve with Glass rod stirring, prepare quality
The glucose solution of mark 5wt%；
(2) it is Si by substrate3N4AFM probe (its SEM figure is shown in Fig. 1) be fixed on syringe needle point, probe tip is in
Front end, is clipped in syringe on contact angle tester, and by observing monitor, it is firm that syringe is slowly moved down into probe tip
Submerge well and the glucose solution in (1) stops, standing 30min；
(3) take out syringe the cone of probe tip kept down and in vacuum drying oven, under the conditions of 60 DEG C, be dried 1h；；
(4) dried probe immersing mass fraction is standing 30min in 90 ~ 98wt% concentrated sulphuric acid；
(5) taking out probe naturally to dry after a small amount of ethanol purge, obtain the AFM probe needle point of carbon coating decoration, its SEM figure is shown in
Fig. 2.
Embodiment 4
Use following steps that atomic force microscope (AFM) probe tip carries out carbon coating decoration:
(1) weigh 0.03g glucose to be dissolved in 0.97mL deionized water, make it dissolve with Glass rod stirring, prepare quality
The glucose solution of mark 3wt%；
(2) it is Si by substrate3N4AFM probe be directly immersed in the glucose solution in (1), stand 30min, take out；
(3) probe taken out is dried in vacuum drying oven 1h under the conditions of 60 DEG C；
(4) dried probe immersing mass fraction is standing 30min in 90 ~ 98wt% concentrated sulphuric acid；
(5) take out probe naturally to dry after a small amount of ethanol purge.
Embodiment 5
Use the Si of unmodified3N4The Si of the method modified of needle point and embodiment 33N4High starch breeding is carried out by needle point respectively
Scanning is to obtain morphology characterization figure, respectively shown in Fig. 3 and Fig. 4, by contrasting it appeared that Fig. 3 entirety more even uniform,
And Fig. 4 demonstrates that color exists certain change, i.e. shows the change of active force.It is found that through modifying and the spy of unmodified
Pin has difference when measuring high starch breeding surface topography, carries out surface sweeping with the probe after modifying, it is possible to obtain more thin
Joint feature.After modified, surface topography depth degree also can change, it was demonstrated that there is active force and changes, but basic feature
Will not change, which ensure that the integrity of measurement.
Thus may certify that, the Si of modified3N4Needle point ensure that original Si3N4On the basis of the function of needle point, permissible
Obtaining new performance, this is that the research of material surface performance has highly important meaning.
The above embodiment of the present invention is only for example of the present invention is described, and is not the enforcement to the present invention
The restriction of mode.For those of ordinary skill in the field, can also be made other not on the basis of the above description
Change and variation with form.Here cannot all of embodiment be given exhaustive.Every belong to technical scheme
That is amplified out obviously changes or changes the row still in protection scope of the present invention.
Claims (8)
1. an atomic force microscope probe tip modification method, it is characterised in that comprise the following steps:
1) aqueous solution of dissolved organic matter is prepared；
2) AFM probe is immersed and the aqueous solution of step 1) preparation stands 30min；
3) AFM probe described in taking-up, is placed under set environment and is dried 1 ~ 2h；
4) dried AFM probe is immersed standing 30min in dehydration carburization agent；
5) AFM probe is taken out, and with ethanol purge, be subsequently placed under atmospheric environment and be dried to constant weight, i.e. obtain carbon cladding and repair
The AFM probe needle point of decorations.
Atomic force microscope probe tip modification method the most according to claim 1, it is characterised in that step 1) preparation
The aqueous solution of dissolved organic matter be mass fraction be the D/W of 3 ~ 5wt%.
Atomic force microscope probe tip modification method the most according to claim 1, it is characterised in that described in step 4)
Dehydration carburization agent be mass fraction be the concentrated sulphuric acid of 90 ~ 98wt%.
Atomic force microscope probe tip modification method the most according to claim 1, it is characterised in that described in step 3)
The vacuum drying oven that set environment is 60 DEG C, drying time is 1h.
Atomic force microscope probe tip modification method the most according to claim 1, it is characterised in that described in step 3)
Set environment be atmosphere at room temperature environment, drying time is 2h.
Atomic force microscope probe tip modification method the most according to claim 4, it is characterised in that step 2) operation
For: AFM probe is fixed on syringe needle point, makes described AFM probe needle point be in foremost, syringe is clipped in contact angle
On tester, make syringe be moved down into AFM probe needle point submerge step 1) preparation aqueous solution in and stand 30min.
Atomic force microscope probe tip modification method the most according to claim 6, it is characterised in that the operation of step 3)
For: take out syringe, make described AFM probe needle point keep down, be placed in the vacuum drying oven of 60 DEG C and be dried 1h.
8. according to the arbitrary described atomic force microscope probe tip modification method of claim 1-7, it is characterised in that described
AFM probe be substrate be Si3N4AFM probe.
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| CN201610587721.6A CN106290989B (en) | 2016-07-25 | 2016-07-25 | A kind of atomic force microscope probe tip modification method |
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| CN201610587721.6A CN106290989B (en) | 2016-07-25 | 2016-07-25 | A kind of atomic force microscope probe tip modification method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107015029A (en) * | 2017-05-11 | 2017-08-04 | 四川理工学院 | AFM contact mode characterizes the method for production with carbon materials sample |
| CN107043929A (en) * | 2017-03-23 | 2017-08-15 | 中国科学院化学研究所 | A kind of method for generating the coat of metal in atomic force microscope probe surface zone of control |
| CN108375687A (en) * | 2018-03-09 | 2018-08-07 | 北京协同创新研究院 | A method of the coated graphite alkene on atomic force microscope probe needle point |
| CN108398578A (en) * | 2018-01-15 | 2018-08-14 | 大连理工大学 | A method of using modified by magnetic nanoparticles atomic force microscope probe |
| 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 |
| CN113219211A (en) * | 2021-04-28 | 2021-08-06 | 西安交通大学 | Preparation method of nano probe |
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| CN107043929A (en) * | 2017-03-23 | 2017-08-15 | 中国科学院化学研究所 | A kind of method for generating the coat of metal in atomic force microscope probe surface zone of control |
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| CN106290989B (en) | 2019-04-12 |
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