CN109521227A - A kind of fast preparation method and application of colloid probe - Google Patents
A kind of fast preparation method and application of colloid probe Download PDFInfo
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- CN109521227A CN109521227A CN201811225545.7A CN201811225545A CN109521227A CN 109521227 A CN109521227 A CN 109521227A CN 201811225545 A CN201811225545 A CN 201811225545A CN 109521227 A CN109521227 A CN 109521227A
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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 fast preparation method of colloid probe and applications: material clean；The dispersion of colloid bead；Tree lace prepares；Probe spreading glue；Colloid probe preparation；For studying the relationship between colloid micro ball and glass plate between contactless force, colloid probe and the aerial F-D curve of glass plate are obtained.The present invention, in conjunction with the tri-axial motion controller of AFM, realizes the gluing of probe and is situated between and see the accurate positionin bonding of particle and probe, to efficiently quickly realize colloid probe preparation using just/inverted light imaging system AFM is equipped with.
Description
Technical field
The present invention relates to precision instrument and colloidal sciences, and more specifically, it relates to a kind of the quick of colloid probe
Preparation method and application.
Background technique
Atomic force microscope (Atomic Force Microscope, AFM) is 1986 by the laboratory IBM Gerd
Two scientist's inventions of Binning and Heinrich Rohrer, they have started a kind of completely new observed pattern, so as to
For people deeper into observation sample surfaces and near-surface region pattern, electricity, the physical characteristics such as mechanics provide atom level
Resolution ratio [Binnig G, Quate C F, Gerber C.Atomic force microscope [J] .Physical review
letters,1986,56(9):930.].The probe of atomic force microscope is generally made of needle point, micro-cantilever and matrix.Needle point is
One key component of probe, it directly determines the resolution ratio of AFM, and testing it quality and application field has important shadow
It rings.Therefore, the continuous development of tip modification and processing technology and improve be particularly important.
Colloid probe technology is by Ducker and Senden et al. earliest in proposition [Ducker WA, Senden in 1991
T J,Pashley R M.Direct measurement of colloidal forces using an atomic force
Microscope [J] .nature, 1991,353 (6341): 239.], it is a kind of by colloidal solid (mainly 0.1-10um
Meso-scale) modification makes to a kind of Jie sight on the needle point of atomic force microscope probe and application technology.It is for studying glue
Body particle (including particulate matter, bacterium, frustule etc.), micro-nano friction, Double layer force, surface potential stick in vapour/liquid phase
Power, Young's modulus measurement and soft substance morphology characterization etc., plays a significant role.
In general, the preparation method of colloid probe mainly has Double-Line Method, micro-pipe cantilever draws method and micro-cantilever method.Traditional is double
Collimation method needs two very thin metal wires to carry out the running fix and particle bonding of colloidal solids, there is that process is tedious, easy to pollute
Sample surfaces and damage probe, it is insufficient that efficiency and success rate are low etc..Although it is accurate quickly that micro-pipe cantilever draws method, technology is also
Its still immature probe is expensive, is unfavorable for generally using.Most common micro-cantilever method, applies in general to larger colloid
The preparation (30-200um) of probe, the preparation for seeing particle probe to 0.2-30um Jie is also highly difficult, is of limited application.
Aiming at the problem that the existing colloid probe technology of preparing means scarcity in China and low efficiency, establish a kind of simple, quick
Effective colloid probe preparation method, to the development important in inhibiting of colloid science and related fields.
Summary of the invention
Purpose of the invention is to overcome the shortcomings in the prior art, proposes a kind of more convenient, simple, effective colloid
The fast preparation method and application of probe, using just/inverted light imaging system AFM is equipped with, in conjunction with the three-axis moving control of AFM
Device processed realizes the gluing of probe and is situated between and see the accurate positionin bonding of particle and probe, to efficiently quickly realize colloid probe
Preparation.
The purpose of the present invention can be achieved through the following technical solutions.
The fast preparation method of colloid probe of the invention, comprising the following steps:
Step 1: material clean
18*18*2mm sheet glass is sequentially placed into ultrapure water, acetone and ultrapure water, is cleaned by ultrasonic 10 minutes respectively, with
Sufficiently removal surface contaminant, is then dried for standby, obtains sheet glass G；
Step 2: colloid bead disperses
By suitable clean microballoon in suitable dispersions liquid, ultrasonic 1-5 minutes makes microballoon be uniformly dispersed；It is taken with pipettor suitable
Amount mixing drop is in the sheet glass G1 cleaned；Confirm that microballoon is uniformly dispersed in AFM optical system, medium density；It is heating
Suitably heating makes sheet glass on plate, accelerates dispersion liquid volatilization, and dry microspheres are uniformly covered with the sheet glass G2 of microballoon；
Step 3: tree lace prepares
It takes suitable glue drop on a clean sheet glass, the tree lace of appropriate thickness is marked with filament, obtain band glue
The sheet glass G3 of line；
Step 4: probe spreading glue
Probe to be finished is loaded onto, AFM laser point is adjusted, makes front end and reflected intensity conjunction of the laser irradiation in probe cantilever
It is suitable, to guarantee that knit stitch is smooth；Z axis is declined into certain position, finds suitable tree lace position, positioning probe viscose glue point, directly into
Needle stops 30 seconds after inserting needle success, lifts needle, probe has applied glue at this time；
Step 5: prepared by colloid probe
Z axis is recalled completely, removes sheet glass G3, changes sheet glass G2；With the 4th step, Z axis is declined into certain position to energy
Enough observe the bead of slide surface, then positioning probe cantilever top, direct inserting needle stops 30 seconds after inserting needle success, lift
Needle, cantilever top has been stained with bead at this time.
Sheet glass described in the first step can be replaced quartz plate or mica sheet or silicon wafer.
Acetone described in the first step can be replaced ethyl alcohol or methanol or acetonitrile.
Microballoon described in second step be polystyrene microsphere or silicon dioxide microsphere or glass microsphere or aluminum oxide micro-sphere or
Zirconium oxide microballoons or zinc sulphide microballoon, microspherulite diameter range is in 0.2-30um.
AFM described in second step should have optical imaging system, and AFM selects Park NX12 or Park NX10 or MFP-3D
Or AFM equipment of Bruker Resolve or Bruker the dimension icon or other with high power imaging system.
Glue described in third step is HARDMANAB glue or PattexAB glue or DELI AB glue or other bonds microballoon
Glue with curing time of probe at 3-60 minutes.
Probe described in 4th step uses the probe with needle point or the probe without needle point, and probe is set as rectangle or V-arrangement.
The purpose of the present invention can be also achieved through the following technical solutions.
The application of alternate probe based on above method preparation of the invention, it is non-between colloid micro ball and glass plate for studying
Relationship between contact force obtains colloid probe and the aerial F-D curve of glass plate, the specific steps are as follows:
Step 1: AFM parametric calibration
Freshly prepd colloid probe is loaded onto, debugging AFM calibrates probe parameter, including " Sensitivity ", " Force
Slope " and " Force constant "；
Step 2: test base prepares
Select roughness less than 100nm 15*15mm cleaning sheet glass be used as base, into/lift needle speed be set as 1.0um/s,
It is tested at room temperature；
Step 3: F-D curve in test air
With between colloid probe and glass plate closer and farther from process, pass through the deformation of AFM cantilever beam and the piezoelectricity system of AFM
System obtains the relationship of distance and voltage change；Power is calculated by the relationship between voltage change and the size of power and apart from it
Between variation relation, to obtain colloid probe and the aerial F-D curve of glass plate.
Compared with prior art, the beneficial effects brought by the technical solution of the present invention are as follows:
The fast preparation method of colloid probe of the invention, the high power imaging system and high-precision being directly equipped with AFM
Three-axis control system, to prepare colloid probe.It is more convenient compared with traditional Double-Line Method, reduce quilt in probe preparation process
The probability of pollution or damage, can effectively improve the power that is prepared into colloid probe, and preparation process is simple, and preparation efficiency is high；With
Micro-cantilever is drawn method and is compared, and more economically, reduces colloid probe preparation to the dependence of expensive instrument, is suitble to extensive promote
Using；Compared with traditional micro-cantilever method, the imaging system of high power is equipped with, it can be achieved that being situated between to 2-30um and sees the preparation of particle probe,
Effectively expand the application and research range of colloid probe.Therefore this preparation method have it is succinct it is quick, at low cost, have a wide range of application
The features such as.
Detailed description of the invention
Fig. 1 is the flow diagram that the present invention prepares colloid probe with AFM；
Fig. 2 is that microballoon adheres to result figure on probe under the microscope for the colloid probe for preparing in embodiment 1；
Fig. 3 is colloid probe and the aerial F-D curve graph of glass plate in embodiment 2.
Specific embodiment
The fast preparation method of colloid probe according to the present invention further illustrates implementation process in conjunction with attached drawing.
The fast preparation method of colloid probe of the invention, the modification and preparation for being related to atomic force microscope colloid probe add
Work method.By the microballoon of meso-scale, the high power imaging system and high-precision three-axis control system being directly equipped with AFM are come
Colloid probe is prepared, and is used for the test of power-distance (F-D) curve in environment micro-interface field.As shown in Figure 1, specific
Realization process is as follows:
Step 1: material clean
If dry plate 18*18*2mm sheet glass is sequentially placed into ultrapure water, acetone and ultrapure water, it is cleaned by ultrasonic 10 points respectively
Then clock is dried for standby with sufficiently removing surface contaminant, obtain sheet glass G.Wherein, acetone can be replaced ethyl alcohol or methanol
Or acetonitrile.Sheet glass can be replaced quartz plate or mica sheet or silicon wafer.
Step 2: colloid bead disperses
By suitable clean microballoon in suitable dispersions liquid, ultrasonic 1-5 minutes makes microballoon be uniformly dispersed；It is taken with pipettor suitable
Amount mixing drop is in the sheet glass G1 cleaned；Confirm that microballoon is uniformly dispersed in AFM optical system, medium density.Then, exist
Suitably heating makes sheet glass in heating plate, accelerates dispersion liquid volatilization, and dry microspheres are uniformly covered with the sheet glass G2 of microballoon.
Wherein, polystyrene microsphere or silicon dioxide microsphere or glass microsphere or aluminum oxide micro-sphere can be used in the microballoon or zirconium oxide is micro-
Ball or zinc sulphide microballoon, microspherulite diameter range is in 0.2-30um.Atomic force microscope (AFM) should have optical imaging system, AFM
Can be selected Park NX12 or Park NX10 or MFP-3D or Bruker Resolve or Bruker dimension icon or its
Its AFM equipment with high power imaging system.
Step 3: tree lace prepares
It takes suitable glue drop on a clean sheet glass, tree lace (the best non-company of appropriate thickness is marked with filament
It is continuous), obtain the sheet glass G3 with tree lace.Wherein, HARDMAN AB glue or PattexAB glue or DELI can be used in glue used
The glue of AB glue or other curing times for bonding microballoon and probe at 3-60 minutes.
Step 4: probe spreading glue
Probe to be finished is loaded onto, AFM laser point is adjusted, makes front end and reflected intensity conjunction of the laser irradiation in probe cantilever
It is suitable, to guarantee that knit stitch is smooth；Z axis is declined into certain position, finds suitable tree lace position, positioning probe viscose glue point, directly into
Needle stops 30 seconds after inserting needle success, lifts needle, probe has applied glue at this time.Wherein, band needle can be used in the probe of AFM used
Sharp probe or the probe without needle point, probe may be configured as rectangle or V-arrangement.
Step 5: prepared by colloid probe
Z axis is recalled completely, removes sheet glass G3, changes sheet glass G2.With the 4th step, Z axis is declined into certain position to energy
Enough observe the bead of slide surface, then positioning probe cantilever top, direct inserting needle stops 30 seconds after inserting needle success, lift
Needle, cantilever top has been stained with bead at this time.
The application of alternate probe based on above method preparation of the invention, it is non-between colloid micro ball and glass plate for studying
Relationship between contact force obtains colloid probe and the aerial F-D curve of glass plate, the specific steps are as follows:
Step 1: AFM parametric calibration
Freshly prepd colloid probe is loaded onto, debugging AFM calibrates probe parameter, including " Sensitivity ", " Force
Slope " and " Force constant ".
Step 2: test base prepares
Select roughness less than 100nm 15*15mm cleaning sheet glass be used as base, into/lift needle speed be set as 1.0um/s,
It is tested at room temperature, Detailed Experimental process can be referring to [Assemi S, Nalaskowski J, Johnson W P.Direct
force measurements between carboxylate-modified latex microspheres and glass
using atomic force microscopy[J].Colloids and Surfaces A:Physicochemical and
EngineeringAspects,2006,286(1-3):70-77.]。
Step 3: F-D curve in test air
With between colloid probe and glass plate closer and farther from process, pass through the deformation of AFM cantilever beam and the piezoelectricity system of AFM
System obtains the relationship of distance and voltage change；Power is calculated by the relationship between voltage change and the size of power and apart from it
Between variation relation, to obtain colloid probe and the aerial F-D curve of glass plate.
Embodiment 1
1. substrate material cleans.1 18*18*2mm sheet glass is sequentially placed into ultrapure water, acetone and ultrapure water, respectively
Ultrasonic cleaning 10 minutes, sufficiently to remove surface contaminant, is then dried for standby, obtains sheet glass G.
2. colloidal solution dilutes.It is 4.99 × 10 by concentration8Particles/ml, partial size are that the polystyrene of 4.5um is small
Ball stoste A is diluted in ultrapure water, and obtaining concentration is 2.50 × 106The dispersion liquid B of particles/ml.
3. colloid bead disperses.20uL dispersion liquid B drop side on the sheet glass G1 cleaned is taken with pipettor, is such as schemed
In 1 shown in (a).
4. dispersion liquid is dry.On hot plate, in the case of 40 DEG C, appropriate heating makes sheet glass, accelerates dispersion liquid volatilization, does
Dry microballoon is uniformly covered with the sheet glass G2 of microballoon, as shown in figure 1 shown in (b).
5.AFM fills needle.Probe TL-COUNT to be finished is loaded onto, AFM laser point is adjusted, keeps laser irradiation outstanding in probe
The front end of arm and reflected intensity is suitable, to guarantee that knit stitch is smooth.
6. tree lace prepares.Equivalent PattexA glue and B glue are taken, is uniformly mixed for use on another clean sheet glass G0, then uses
The copper wire of one diameter 0.3mm glues appropriate glue from G0, draws tree lace in the side of the not dispersed globules of sheet glass G2, obtains glass
Piece G3, as shown in figure 1 shown in (c).
7. probe cementing.Sheet glass G3 is put in AFM test base；The three-axis control system for adjusting AFM, will be under Z axis
Certain position is dropped, suitable tree lace position, positioning probe viscose glue point are found, direct inserting needle stops 30 seconds after inserting needle success, lift
Needle, probe has applied glue at this time, as shown in figure 1 shown in (d).
8. probe glues microballoon.The probe for being stained with glue is recalled into Z axis completely, adjusts the three-axis control system of AFM, by Z axis
Decline certain position, find suitable microballoon position, as shown in figure 1 shown in (e).Same step (7), extremely by Z axis decline certain position
It can observe the bead of glass sheet surface, then right above positioning probe cantilever top to bead, direct inserting needle, inserting needle success
Afterwards, it stops 30 seconds, lifts needle, cantilever top has been stained with bead at this time, as shown in figure 1 shown in (f).
9. probe is stained with microballoon confirmation.The colloid probe of preparation is removed and adheres to spy with the micro- sem observation microballoon of research grade
On needle, as a result as shown in Figure 2.
As shown in Figure 2, successfully TL-COUNT tipless cantilever tip, modification are arrived in modification to the polystyrene microsphere of 4.5um
The position suitable of bonding can carry out the relevant test job of colloid probe after well-bonded
Embodiment 2
According to TL-COUNT probe prepared by embodiment 1, the research of contactless force between colloid micro ball and glass plate is carried out, is adopted
F-D curve is tested with the Contact mode of ParkNX10AFM, the specific steps are as follows:
1.AFM parametric calibration.Freshly prepd colloid probe is loaded onto, debugging AFM calibrates probe parameter, including
" Sensitivity ", " Force slope " and " Force constant ".By calibration obtain " Sensitivity " and
" Force constant " is respectively 4.1V/um and 10-3(N/m)。
2. testing base to prepare.Select 15*15mm cleaning sheet glass of the roughness less than 100nm as base, into/lift needle
Speed is set as 1.0um/s, is tested at room temperature, Detailed Experimental process can referring to [Assemi S, Nalaskowski J,
Johnson W P.Direct force measurements between carboxylate-modified latex
microspheres and glass using atomic force microscopy[J].Colloids and Surfaces
A:Physicochemical and Engineering Aspects,2006,286(1-3):70-77.]。
3. testing F-D curve in air.With between colloid probe and glass plate closer and farther from process, pass through AFM cantilever
The deformation of beam and the piezoelectric system of AFM obtain the relationship of distance and voltage change.By between voltage change and the size of power
The variation relation between power and distance is calculated in relationship, so that colloid probe and the aerial F-D curve of glass plate are obtained,
As a result as shown in Figure 3.
From the figure 3, it may be seen that using colloid probe prepared by the present invention can to the contactless force between microballoon and glass base into
Row measurement.Need colloid probe prepare and correlation AFM test job in, compared with traditional Double-Line Method, this method more rapidly,
It is more simple and easy.
Although function and the course of work of the invention are described above in conjunction with attached drawing, the invention is not limited to
Above-mentioned concrete function and the course of work, the above mentioned embodiment is only schematical, rather than restrictive, ability
The those of ordinary skill in domain under the inspiration of the present invention, is not departing from present inventive concept and scope of the claimed protection situation
Under, many forms can also be made, all of these belong to the protection of the present invention.
Claims (8)
1. a kind of fast preparation method of colloid probe, which comprises the following steps:
Step 1: material clean
18*18*2mm sheet glass is sequentially placed into ultrapure water, acetone and ultrapure water, is cleaned by ultrasonic 10 minutes respectively, with abundant
Surface contaminant is removed, is then dried for standby, obtains sheet glass G；
Step 2: colloid bead disperses
By suitable clean microballoon in suitable dispersions liquid, ultrasonic 1-5 minutes makes microballoon be uniformly dispersed；It is taken with pipettor appropriate mixed
Drop is closed in the sheet glass G1 cleaned；Confirm that microballoon is uniformly dispersed in AFM optical system, medium density；On hot plate
Appropriate heating makes sheet glass, accelerates dispersion liquid volatilization, and dry microspheres are uniformly covered with the sheet glass G2 of microballoon；
Step 3: tree lace prepares
It takes suitable glue drop on a clean sheet glass, the tree lace of appropriate thickness is marked with filament, is obtained with tree lace
Sheet glass G3；
Step 4: probe spreading glue
Load onto probe to be finished, adjust AFM laser point, make laser irradiation probe cantilever front end and reflected intensity it is suitable,
To guarantee that knit stitch is smooth；Z axis is declined into certain position, finds suitable tree lace position, positioning probe viscose glue point, direct inserting needle,
It after inserting needle success, stops 30 seconds, lifts needle, probe has applied glue at this time；
Step 5: prepared by colloid probe
Z axis is recalled completely, removes sheet glass G3, changes sheet glass G2；With the 4th step, Z axis decline certain position can extremely be seen
The bead of slide surface being measured, then positioning probe cantilever top, direct inserting needle stops 30 seconds after inserting needle success, needle is lifted,
Cantilever top has been stained with bead at this time.
2. the fast preparation method of colloid probe according to claim 1, which is characterized in that sheet glass described in the first step
It can be replaced quartz plate or mica sheet or silicon wafer.
3. the fast preparation method of colloid probe according to claim 1, which is characterized in that acetone described in the first step can
Replace with ethyl alcohol or methanol or acetonitrile.
4. the fast preparation method of colloid probe according to claim 1, which is characterized in that microballoon described in second step is
Polystyrene microsphere or silicon dioxide microsphere or glass microsphere or aluminum oxide micro-sphere or zirconium oxide microballoons or zinc sulphide microballoon, microballoon
Particle size range is in 0.2-30um.
5. the fast preparation method of colloid probe according to claim 1, which is characterized in that AFM described in second step is answered
With optical imaging system, AFM selects Park NX12 or Park NX10 or MFP-3D or Bruker Resolve or Bruker
AFM equipment of the dimension icon or other with high power imaging system.
6. the fast preparation method of colloid probe according to claim 1, which is characterized in that glue described in third step is
HARDMANAB glue or PattexAB glue or DELI AB glue or other curing times for bonding microballoon and probe were at 3-60 minutes
Glue.
7. the fast preparation method of colloid probe according to claim 1, which is characterized in that probe described in the 4th step is adopted
With the probe with needle point or without the probe of needle point, probe is set as rectangle or V-arrangement.
8. a kind of application of the alternate probe based on the preparation of claim 1 to 7 the method, which is characterized in that for studying glue
Relationship between body microballoon and glass plate between contactless force obtains colloid probe and the aerial F-D curve of glass plate, specifically
Steps are as follows:
Step 1: AFM parametric calibration
Freshly prepd colloid probe is loaded onto, debugging AFM calibrates probe parameter, including " Sensitivity ", " Force slope "
" Force constant "；
Step 2: test base prepares
Select roughness less than 100nm 15*15mm cleaning sheet glass be used as base, into/lift needle speed be set as 1.0um/s, room temperature
Under tested；
Step 3: F-D curve in test air
With between colloid probe and glass plate closer and farther from process, obtained by the deformation of AFM cantilever beam and the piezoelectric system of AFM
To the relationship of distance and voltage change；It is calculated between power and distance by the relationship between voltage change and the size of power
Variation relation, to obtain colloid probe and the aerial F-D curve of glass plate.
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| CN110658361A (en) * | 2019-09-27 | 2020-01-07 | 北京航空航天大学 | Mechanical response measuring tool based on Atomic Force Microscope (AFM) scanning probe |
| CN111505345A (en) * | 2020-05-15 | 2020-08-07 | 大连理工大学 | Atomic force microscope probe modification method based on scanning electron microscope micro-control system |
| WO2021114789A1 (en) * | 2019-12-11 | 2021-06-17 | 浙江大学 | Biomembrane force probe system-based super-alignment force clamp experimental method |
| CN113267649A (en) * | 2021-04-29 | 2021-08-17 | 大连海事大学 | Preparation method of long-arm probe of atomic force microscope |
| CN114280333A (en) * | 2021-03-25 | 2022-04-05 | 华侨大学 | Method for testing adhesion of superfine abrasive and semiconductor wafer |
| CN114578098A (en) * | 2022-01-21 | 2022-06-03 | 西安理工大学 | Method for preparing colloid probe in atomic force microscope |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110658361A (en) * | 2019-09-27 | 2020-01-07 | 北京航空航天大学 | Mechanical response measuring tool based on Atomic Force Microscope (AFM) scanning probe |
| WO2021114789A1 (en) * | 2019-12-11 | 2021-06-17 | 浙江大学 | Biomembrane force probe system-based super-alignment force clamp experimental method |
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| CN114280333A (en) * | 2021-03-25 | 2022-04-05 | 华侨大学 | Method for testing adhesion of superfine abrasive and semiconductor wafer |
| CN113267649A (en) * | 2021-04-29 | 2021-08-17 | 大连海事大学 | Preparation method of long-arm probe of atomic force microscope |
| CN114578098A (en) * | 2022-01-21 | 2022-06-03 | 西安理工大学 | Method for preparing colloid probe in atomic force microscope |
| CN114578098B (en) * | 2022-01-21 | 2023-09-22 | 西安理工大学 | Method for preparing colloid probe in atomic force microscope |
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