CN108398579A - A kind of chemical force microscopes technology probe and preparation method thereof - Google Patents
A kind of chemical force microscopes technology probe and preparation method thereof Download PDFInfo
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- CN108398579A CN108398579A CN201810305816.3A CN201810305816A CN108398579A CN 108398579 A CN108398579 A CN 108398579A CN 201810305816 A CN201810305816 A CN 201810305816A CN 108398579 A CN108398579 A CN 108398579A
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- gold
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- 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 chemical force microscopes technology probes and preparation method thereof.The probe includes that gold-plated atomic force microscope probe and monomolecular adsorption layer form；The gold-plated atomic force microscope probe is that atomic force microscope probe surface coats gold-plated basal layer；The monomolecular adsorption layer is that decorating molecule is formed with the gold-plated basal layer by golden sulfur bond.The present invention uses the chemical modification of the method detecting probe surface of unimolecule self assembly, this method that can form different monomolecular adsorption layers using golden sulfide linkage in gold-plated surface；Can the characteristic group of the molecule to being modified as needed be adjusted；It is used for the adherency force effect between the special substrate of quantitative measurment and specific function needle point using the present invention；Realize that the direct in-situ for characteristic group's intermolecular interaction measures.This method is easy to operate, at low cost, environmentally protective, can meet general industry production requirement.
Description
Technical field
The present invention relates to a kind of chemical force microscopes technology probes and preparation method thereof, belong to atomic force microscope mechanics and answer
Use field.
Background technology
((self-assembled monolayers, abbreviation SAMs technology) is by molecule spy to unimolecule self-assembling technique
Chemisorption is very generated between end group and substrate, and orderly molecule assembled layers are spontaneously formed on interface.It has in situ spontaneous
The advantages that formation, higher order and orientation, high density are accumulated, defect is few and stable structure.In scientific research and life
The numerous areas such as production, life have extremely wide application prospect.
Invention content
The object of the present invention is to provide a kind of chemical force microscopes technology probe and preparation method thereof, the method for the present invention operations
Simply, at low cost, it is environmentally protective, general industry production requirement can be met.
A kind of chemical force microscopes technology probe provided by the invention, which includes atomic force microscope probe, gold-plated
Basal layer and monomolecular adsorption layer composition；
The atomic force microscope probe surface coats the gold-plated basal layer；
The monomolecular adsorption layer is that decorating molecule is formed with the gold-plated basal layer by gold-sulfur bond.
In above-mentioned probe, the decorating molecule is that sulfydryl is contained in one end in structural formula, and the other end contains characteristic group
Characteristic molecular.
In above-mentioned probe, the skeleton symbol of the decorating molecule is shown in following formula I,
HS-(CH2)n- R formulas I；
In formula I, R is at least one of amino, carboxyl, methyl and phenyl；
The natural number that n is 1~18.
In above-mentioned probe, the thickness of the gold-plated basal layer is 50~70nm.
In the present invention, the base material of the gold-plated basal layer is material well known to ability, and the gold-plated basal layer is specific
It can be gold plate.
Chemical force microscopes technology probe of the present invention can the characteristic group of the molecule to being modified as needed adjust
Section；It can be used for the adherency force effect between the special substrate of quantitative measurment and specific function needle point using the present invention；Realization is directed to
The direct in-situ of characteristic group's intermolecular interaction measures.
The present invention also provides a kind of preparation methods of chemical force microscopes technology probe, include the following steps：It will be gold-plated
Atomic force microscope probe impregnated in the solution of the decorating molecule, then take out dry to get to chemical force microscopes
Technology probe.
In above-mentioned preparation method, at least one of etoh solvent, toluene and acetone of the solution of the decorating molecule.
In above-mentioned preparation method, the concentration of the solution of the molecule to be finished can be 2~5mM.
In above-mentioned preparation method, the time of the immersion can be 18~36h, concretely for 24 hours.
The present invention has the following advantages：
The present invention realizes that the chemistry of atomic force microscope (abbreviation AFM) detecting probe surface is repaiied using the method for unimolecule self assembly
Decorations, this method can form different monomolecular adsorption layers using golden sulfide linkage in gold-plated surface.Chemical force of the present invention is aobvious
Micromirror technologies (abbreviation CFM) can the characteristic group of the molecule to being modified as needed be adjusted；Utilize energy of the present invention
For the adherency force effect between the special substrate of quantitative measurment and specific function needle point；It realizes intermolecular for characteristic group
The direct in-situ of interaction force measures.This method is easy to operate, at low cost, environmentally protective, can meet general industry production and want
It asks.
Description of the drawings
Fig. 1 is that one end used in the embodiment of the present invention 1 is sulfydryl, and the other end is the modification special molecular structure of amino
Formula.
Fig. 2 is that the present invention implements CFM probe schematic diagrames obtained, and wherein Fig. 2 (a) is that the embodiment of the present invention 1 is prepared
, Fig. 2 (b) is what the embodiment of the present invention 2 was prepared, and Fig. 2 (c) is what the embodiment of the present invention 3 was prepared, and Fig. 2 (d) is this
What inventive embodiments 4 were prepared.
Fig. 3 is gold-plated surface modification-NH made from the embodiment of the present invention 12XPS spectrum figure afterwards.
Fig. 4 is that the comparison of functionalized surface contact angle is made in the static contact angle of the water of gold-plated surface and the embodiment of the present invention 1,
Wherein Fig. 4 (a) is the static contact angle of the water of gold-plated surface, and Fig. 4 (b) is that functionalized surface contact is made in the embodiment of the present invention 1
Angle.
Fig. 5 is the CFM needle points adherency that functionalization is made with the embodiment of the present invention 1 for adhesion strength between common afm tip and substrate
The common adhesion strength between afm tip and substrate of the comparison of power, wherein Fig. 5 (a), Fig. 5 (b) are that functionalization is made in the embodiment of the present invention 1
CFM needle point adhesion strengths comparison.
Fig. 6 is that one end used in the embodiment of the present invention 2 is sulfydryl, and the other end is the modification special molecular structure of carboxyl
Formula.
Fig. 7 is that the comparison of functionalized surface contact angle is made in the static contact angle of the water of gold-plated surface and the embodiment of the present invention 2,
Wherein Fig. 7 (a) is the static contact angle of the water of gold-plated surface, and Fig. 7 (b) is that functionalized surface contact is made in the embodiment of the present invention 2
Angle.
Fig. 8 is the CFM needle points adherency that functionalization is made with the embodiment of the present invention 2 for adhesion strength between common afm tip and substrate
The common adhesion strength between afm tip and substrate of the comparison of power, wherein Fig. 8 (a), Fig. 8 (b) are that functionalization is made in the embodiment of the present invention 2
CFM needle point adhesion strengths comparison.
Fig. 9 is that one end used in the embodiment of the present invention 3 is sulfydryl, and the other end is the modification special molecular structure of alkyl
Formula.
Figure 10 is that functionalized surface contact angle pair is made in the static contact angle of the water of gold-plated surface and the embodiment of the present invention 3
Than wherein Figure 10 (a) is the static contact angle of the water of gold-plated surface, and Figure 10 (b) is that functionalized surface is made in the embodiment of the present invention 3
Contact angle.
Figure 11 is the CFM needle points adherency that functionalization is made with the embodiment of the present invention 3 for adhesion strength between common afm tip and substrate
The common adhesion strength between afm tip and substrate of the comparison of power, wherein Figure 11 (a), Figure 11 (b) are that function is made in the embodiment of the present invention 3
The comparison of the CFM needle point adhesion strengths of change.
Figure 12 is that one end used in the embodiment of the present invention 4 is sulfydryl, and the other end is the modification particular molecule knot of phenyl
Structure formula.
Figure 13 is that functionalized surface contact angle pair is made in the static contact angle of the water of gold-plated surface and the embodiment of the present invention 4
Than wherein Figure 13 (a) is the static contact angle of the water of gold-plated surface, and Figure 13 (b) is that functionalized surface is made in the embodiment of the present invention 4
Contact angle.
Figure 14 is the CFM needle points adherency that functionalization is made with the embodiment of the present invention 4 for adhesion strength between common afm tip and substrate
The common adhesion strength between afm tip and substrate of the comparison of power, wherein Figure 14 (a), Figure 14 (b) are that function is made in the embodiment of the present invention 4
The comparison of the CFM needle point adhesion strengths of change.
Specific implementation mode
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
In following embodiments, gold-plated atomic force microscope (AFM) probe is available commercially from Brooker company, and (gold-plated thickness is
50~70nm).
Embodiment 1,
The preparation of particular molecule solution：
It is sulfydryl by one end of 2.39mg, the other end is that the particular molecule of amino is dissolved in 10mL ethyl alcohol, and stirring and dissolving is matched
The ethanol solution of 1mM is made.Special molecular structure formula is as shown in Figure 1.
The preparation of CFM probes：
Gold-plated atomic force microscope (AFM) probe is immersed in structure particular molecule ethanol solution as shown in Figure 1,
Soaking time is 24 hours, the CFM functionalization probes with amino is made, as shown in Fig. 2 (a).
As shown in figure 3, due to constituent content that can not be on direct detection CFM needle points, therefore use plating gold substrate as needle point
Analogies carry out x-ray photoelectron spectroscopy (XPS) and characterize.Gold-plated surface modification amino (- NH made from the embodiment of the present invention2) after
XPS spectrum figure, N element appearance is more apparent as we can see from the figure, show plate gold substrate covered by characteristic group.
As shown in figure 4, the static contact angle of the water of gold-plated surface is 72.0 °, and amino (- NH is modified2) after surface
Water static contact angle be 50.4 °, show that this method can be realized successfully and surface modified using gold-sulfur bond.
Similarly it is found that the modification to afm tip equally may be implemented using this method in gold-plated needle surface, ammonia has been modified to prepare
Base (- NH2) CFM functionalization probes.
As shown in Fig. 5 (a), the adhesion strength between the common afm tip through functional modification and substrate is weaker, and of the invention
Functional modification amino (- NH2) CFM needle points and substrate between adhesion strength (such as Fig. 5 (b)) it is apparent under the same conditions more
By force, this feasibility for also having reconfirmed method of modifying of the present invention, the method for the present invention, which can be realized successfully, utilizes gold-sulfur bond pair
Surface is modified.
Embodiment 2,
The preparation of particular molecule solution：
It is sulfydryl by one end of 2.18mg, the other end is that the particular molecule of carboxyl is dissolved in 10mL ethyl alcohol, and stirring and dissolving is matched
The ethanol solution of 1mM is made.The structural formula of particular molecule is as shown in Figure 6.
The preparation of CFM probes
Atomic force microscope (AFM) probe is impregnated in particular molecule ethanol solution in figure 6, soaking time is 24 small
When, the CFM functionalization probes with carboxyl are made, as shown in Fig. 2 (b).
As shown in fig. 7, the static contact angle of the water of gold-plated surface is 72.0 °, and the surface after carboxyl (- COOH) is modified
Water static contact angle be 41.5 °, show that this method can be realized successfully and surface modified using gold-sulfur bond.
Similarly it is found that the modification to afm tip equally may be implemented using this method in gold-plated needle surface, carboxylic has been modified to prepare
The CFM functionalization probes of base (- COOH).
As shown in Fig. 8 (a), the adhesion strength between the common afm tip through functional modification and substrate is weaker, and functionalization
The adhesion strength (such as Fig. 8 (b)) modified between the CFM needle points of carboxyl (- COOH) and substrate is clearly more powerful under the same conditions, this
Reconfirmed the feasibility of method of modifying of the present invention, the method for the present invention can successfully realize using gold-sulfur bond to surface into
Row modification.
Embodiment 3,
The preparation of particular molecule solution：
It is sulfydryl by one end of 2.86mg, the other end is that the particular molecule of alkyl is dissolved in 10mL ethyl alcohol, and stirring and dissolving is matched
The ethanol solution of 1mM is made.Special molecular structure formula is as shown in Figure 9.
The preparation of CFM probes：
Atomic force microscope (AFM) probe is impregnated in particular molecule ethanol solution in fig.9, soaking time is 24 small
When, the CFM functionalization probes with alkyl are made, as shown in Fig. 2 (c).
As shown in Figure 10, the static contact angle of the water of gold-plated surface is 72.0 °, and has modified alkyl (- CH3) after surface
Water static contact angle be 102.2 °, show that this method can be realized successfully and surface modified using gold-sulfur bond.
Similarly it is found that the modification to afm tip equally may be implemented using this method in gold-plated needle surface, alkane has been modified to prepare
Base (- CH3) CFM functionalization probes.
As shown in Figure 11 (a), the adhesion strength between the common afm tip through functional modification and substrate is weaker, and function
Alkyl (- CH has been modified in change3) CFM needle points and substrate between adhesion strength (such as Figure 11 (b)) it is clearly more powerful under the same conditions, this
Also reconfirmed that the feasibility of method of modifying, the method for the present invention can be realized successfully and be repaiied to surface using gold-sulfur bond
Decorations.
Embodiment 4,
The preparation of particular molecule solution：
It is sulfydryl by one end of 2.50mg, the other end is that the particular molecule of phenyl is dissolved in 10mL ethyl alcohol, and stirring and dissolving is matched
The ethanol solution of 1mM is made.Special molecular structure formula is as shown in figure 12.
The preparation of CFM probes：
Atomic force microscope (AFM) probe is impregnated in particular molecule ethanol solution in fig. 12, soaking time is 24 small
When, band phenyl (- C is made6H5) CFM functionalization probes, as shown in Figure 2.
As shown in figure 13, the static contact angle of the water of gold-plated surface is 72.0 °, and has modified phenyl (- C6H5) after surface
Water static contact angle be 50.4 °, show that this method can be realized successfully and surface modified using gold-sulfur bond.
Similarly it is found that the modification to afm tip equally may be implemented using this method in gold-plated needle surface, benzene has been modified to prepare
Base (- C6H5) CFM functionalization probes.
As shown in Figure 14 (a), the adhesion strength between the common afm tip through functional modification and substrate is weaker, and this hair
Bright functional modification phenyl (- C6H5) CFM needle points and substrate between adhesion strength (such as Figure 14 (b)) it is apparent under the same conditions
Stronger, this has also reconfirmed that the feasibility of method of modifying, the method for the present invention can successfully be realized using gold-sulfur bond to surface
It is modified.
Claims (8)
1. a kind of chemical force microscopes technology probe, it is characterised in that：The probe include gold-plated atomic force microscope probe and
Monomolecular adsorption layer forms；
The gold-plated atomic force microscope probe is that atomic force microscope probe surface coats gold-plated basal layer；
The monomolecular adsorption layer is that decorating molecule is formed with the gold-plated basal layer by gold-sulfur bond.
2. probe according to claim 1, it is characterised in that：The decorating molecule is that sulfydryl is contained in one end in structural formula,
The other end contains the characteristic molecular of characteristic group.
3. probe according to claim 1 or 2, it is characterised in that：The skeleton symbol of the decorating molecule is I institute of following formula
Show,
HS-(CH2)n- R formulas I；
In formula I, R is at least one of amino, carboxyl, alkyl and phenyl；
The natural number that n is 1~18.
4. probe according to any one of claim 1-3, it is characterised in that：The thickness of the gold-plated basal layer be 50~
70nm。
5. a kind of preparation method of chemical force microscopes technology probe, includes the following steps：Gold-plated atomic force microscope is visited
Needle impregnates in the solution of the decorating molecule, then takes out dry to get to chemical force microscopes technology probe.
6. preparation method according to claim 5, it is characterised in that：The etoh solvent of the solution of the decorating molecule, first
At least one of benzene and acetone.
7. preparation method according to claim 5 or 6, it is characterised in that：A concentration of the 2 of the solution of the molecule to be finished
~5mM.
8. according to the preparation method described in any one of claim 5-7, it is characterised in that：The time of the immersion be 18~
36h。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810305816.3A CN108398579A (en) | 2018-04-08 | 2018-04-08 | A kind of chemical force microscopes technology probe and preparation method thereof |
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| CN201810305816.3A CN108398579A (en) | 2018-04-08 | 2018-04-08 | A kind of chemical force microscopes technology probe and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111505343A (en) * | 2020-04-27 | 2020-08-07 | 广西大学 | Method for measuring force curve between zymoprotein and lignin based on AFM probe |
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| JPH06264217A (en) * | 1993-03-15 | 1994-09-20 | Canon Inc | Probe, scanning type probe microscope and information processing device using the probe |
| CN103235158A (en) * | 2013-01-10 | 2013-08-07 | 北京航空航天大学 | Electrochemical atomic force microscope probe carriage-electrolytic cell device |
| CN104360107A (en) * | 2014-11-12 | 2015-02-18 | 苏州大学 | Graphene-clad atomic force microscope probe and manufacturing method and application thereof |
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2018
- 2018-04-08 CN CN201810305816.3A patent/CN108398579A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06264217A (en) * | 1993-03-15 | 1994-09-20 | Canon Inc | Probe, scanning type probe microscope and information processing device using the probe |
| CN103235158A (en) * | 2013-01-10 | 2013-08-07 | 北京航空航天大学 | Electrochemical atomic force microscope probe carriage-electrolytic cell device |
| CN104360107A (en) * | 2014-11-12 | 2015-02-18 | 苏州大学 | Graphene-clad atomic force microscope probe and manufacturing method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| HAN-CHEOL KWON 等: "AFM Force Measurements between SAM-Modified Tip and SAM-Modified Substrate in Alkaline Solution", 《JOURNAL OF PHYSICAL CHEMISTRY B》 * |
| WEI ZHANG 等: "Molecular interactions between DOPA and surfaces with different functional groups: a chemical force microscopy study", 《RSC ADVANCES》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111505343A (en) * | 2020-04-27 | 2020-08-07 | 广西大学 | Method for measuring force curve between zymoprotein and lignin based on AFM probe |
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