CN101256133A - Method for preparing colloid ball sample for three-dimensional calibration of scanning probe microscope - Google Patents
Method for preparing colloid ball sample for three-dimensional calibration of scanning probe microscope Download PDFInfo
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- CN101256133A CN101256133A CNA2008100361625A CN200810036162A CN101256133A CN 101256133 A CN101256133 A CN 101256133A CN A2008100361625 A CNA2008100361625 A CN A2008100361625A CN 200810036162 A CN200810036162 A CN 200810036162A CN 101256133 A CN101256133 A CN 101256133A
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Abstract
The invention belongs to field of the scanning probe microscope technique, particularly relates to a preparing method of colloidal sphere sample which is used for scanning probe microscope three-dimensional calibration. The invention uses improved vertical deposition method, including the following steps: inserting a piece of fresh dissociated mica base-plate vertically into monodispersed colloidal sphere solution at proper concentration, placing the vertical deposition system in the climatic chamber, controlling the temperature and the humidity strictly, until the solution is volatilized totally, then obtaining grating-like shaped mono-layer ordered close-packing colloidal sphere sample, which can be used for calibration of piezoelectric scanning tube of scanning probe microscope along X, Y and Z directions.
Description
Technical field
The invention belongs to the scanning probe microscopy technical field, be specifically related to a kind of preparation method of scan-probe calibration standard sample.
Background technology
Scanning probe microscopy is a kind of novel microcosmic surface analytical instrument that grows up after optical microscope, electron microscope, and it measures character such as the surface topography of tested sample and other electricity, magnetics, mechanics by small probe.For guaranteeing the accuracy of scanning probe microscopy measurement yardstick, must carry out regular calibration to scanning probe microscopy.Used calibration sample mostly is and adopts integrated circuit technology to make at present, has two weak points: the one, and cost height, a general hundreds of of standard specimen even thousands of Renminbi; The 2nd, precision is low, and the size of being demarcated is generally in the micron or the scope of hundreds of nanometer, and along with demarcating reducing of size, the standard specimen cost greatly increases.Therefore develop a kind of scanning probe microscopy with low cost and have high practical value with the preparation method of standard specimen.People such as K.Nagayama have reported on Langmuir periodical (volume was 1303 pages in 1996 the 12nd) and have adopted vertical deposition method to prepare the method for large-area ordered colloidal crystal that this method is mainly used to prepare the colloidal crystal structure of multilayer order.This method is widely adopted in photonic crystal research afterwards.The present invention has done some to people's such as above-mentioned K.Nagayama method and has improved, thereby is used for preparing the class raster-like colloid monolayer ball sample of the three-dimensional calibration of scanning probe microscopy usefulness.
Summary of the invention
The preparation method who the purpose of this invention is to provide the three-dimensional calibration of scanning probe microscope usefulness colloid ball sample that a kind of cost is low, precision is high.
The present invention is a substrate with the fresh mica that dissociates, the fresh mica substrate that dissociates has the flatness of atom level and each is to uniform water wettability, adopt vertical deposition method, by controlling the parameters such as concentration, environment temperature and humidity of single dispersoid ball solution, in the colloid monolayer crystal film of the orderly solid matter of mica substrate surface self assembly one deck class raster-like structure.The periodic structure of colloidal spheres can be used for the calibration of scanning probe microscopy directions X piezoelectric scanning pipe and Y direction piezoelectric scanning pipe in the colloidal crystal film, and the bench height information between colloid monolayer film and the exposed mica substrate can be used for the calibration of Z direction piezoelectric scanning pipe.Concrete preparation process is as follows:
(1) is 0.01-0.02% with monodispersed colloidal spheres solution dilution to mass concentration, and gets colloidal spheres solution and place beaker;
(2) be substrate with the mica, mica is dissociated, vertically insert beaker and be partially submerged in the colloidal spheres solution;
(3) the vertical deposition system is moved in the climatic chamber, and the temperature inside the box and humidity are controlled at appropriate value, temperature is 50 ℃-65 ℃, and humidity is 60%-80%;
(4) colloidal solution volatilization, colloidal spheres is self-assembled into ordered structure at the mica substrate surface;
(5) treat that solution evaporation is intact after, by taking out beaker in the case, take out the mica substrate, can obtain the colloid ball sample of the orderly solid matter of class raster-like individual layer at substrate surface.
With respect to the scanning probe microscopy standard specimen that adopts the integrated circuit technology preparation, preparation method of the present invention is with low cost, and is simple to operate, can prepare the colloid ball sample of particle diameter in 90nm～800nm scope at an easy rate.
Description of drawings
Fig. 1 is the device synoptic diagram of vertical deposition system.
Fig. 2 is the optical photograph of the prepared orderly solid matter colloid ball sample of class raster-like individual layer.Length of the scale is 50 μ m among the figure, wherein, is the individual layer solid matter colloidal film that the vertical deposition method self-assembled growth becomes (a), (b) is the mica substrate that exposes.
Fig. 3 is the scanning probe microscopy photo of orderly solid matter structure on the colloid monolayer film, sweep limit 5 μ m * 5 μ m.
Fig. 4 is the scanning probe microscopy photo of the step between colloid monolayer film and the exposed substrate, sweep limit 5 μ m * 5 μ m, and wherein (a) is colloidal film, (b) is exposed mica substrate.
Number in the figure: 1 is anchor clamps, is used for fixing mica sheet, and 2 is beaker, and 3 are the fresh mica sheet that dissociates, and 4 is liquid level, and 5 is colloidal spheres, and 6 is base.
Embodiment
Below in conjunction with two embodiment, set forth the preparation method of the orderly solid matter colloid ball sample of class raster-like individual layer that the present invention stated.
Monodispersed polystyrene colloid ball aqueous solution is provided, and colloid sphere diameter 238nm is 0.01% with deionized water with solution dilution to mass concentration;
The colloidal spheres solution of getting after 4ml dilutes is inserted in the beaker that nominal capacity is 5ml;
The fresh mica sheet that dissociates is vertically inserted in the beaker, and mica sheet immerses the partly about 2cm of solution;
System puts into climatic chamber with vertical deposition, and the control temperature is 60 ℃, and relative humidity is 74.5%;
After 30 hours, solution volatilizees fully, takes out beaker, takes out mica sheet, can obtain the colloid ball sample of the orderly solid matter of class raster-like individual layer.
Monodispersed polystyrene colloid ball ethanolic solution is provided, and colloid sphere diameter 420nm is 0.015% with absolute ethyl alcohol with solution dilution to mass concentration;
The colloidal spheres solution of getting after 4ml dilutes is inserted in the beaker that nominal capacity is 5ml;
The fresh mica sheet that dissociates is vertically inserted in the beaker, and mica sheet immerses the partly about 2cm of solution;
System puts into climatic chamber with vertical deposition, and the control temperature is 50 ℃, and relative humidity is 74.4%;
After 18 hours, solution volatilizees fully, takes out beaker, takes out mica sheet, can obtain the colloid ball sample of the orderly solid matter of class raster-like individual layer.
In addition, be understandable that, the concentration of solution, colloid sphere diameter, the solvent that is adopted, environment temperature and humidity all can influence the number of plies of prepared colloidal crystal film, in order to obtain the class raster-like colloidal crystal film that the present invention states, tackle the in addition careful regulation and control of these five parameters, and to colloidal film width of fringe and exposed substrate width of fringe in the meticulous adjusting of these five parameters also may command optical grating construction shown in Figure 2.The width of used mica substrate is unsuitable too narrow, generally should be greater than 1.5cm.
Claims (3)
1. a three-dimensional calibration of scanning probe microscope is characterized in that concrete steps are as follows with the preparation method of colloid ball sample:
(1) is 0.01-0.02% with monodispersed colloidal spheres solution dilution to mass concentration, and gets colloidal spheres solution and place beaker;
(2) be substrate with the mica, mica is dissociated, vertically insert beaker and be partially submerged in the colloidal spheres solution;
(3) the vertical deposition system is moved in the climatic chamber, and the temperature inside the box is controlled to be 50 ℃-65 ℃, humidity is controlled to be 60%-80%;
(4) colloidal solution volatilization, colloidal spheres is self-assembled into ordered structure at the mica substrate surface;
(5) treat that solution evaporation is intact after, by taking out beaker in the case, take out the mica substrate, can obtain the colloid ball sample of the orderly solid matter of class raster-like individual layer at substrate surface.
2. preparation method as claimed in claim 1 is characterized in that described colloid sphere diameter is between 90nm～800nm.
3. preparation method as claimed in claim 1 is characterized in that the solvent of using in the described colloidal spheres solution is deionized water or absolute ethyl alcohol.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008100361625A CN101256133A (en) | 2008-04-17 | 2008-04-17 | Method for preparing colloid ball sample for three-dimensional calibration of scanning probe microscope |
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| CNA2008100361625A CN101256133A (en) | 2008-04-17 | 2008-04-17 | Method for preparing colloid ball sample for three-dimensional calibration of scanning probe microscope |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103018492A (en) * | 2012-11-21 | 2013-04-03 | 西安建筑科技大学 | Device and method for preparing PVDF (polyvinylidene fluoride) micro-particle probe by physical adhesion method |
| CN103018493A (en) * | 2012-11-21 | 2013-04-03 | 西安建筑科技大学 | Device and method for preparing PVDF (polyvinylidene fluoride) microparticle probe by using melting-sintering method |
| RU2481590C2 (en) * | 2010-08-17 | 2013-05-10 | Закрытое Акционерное Общество "Нанотехнология Мдт" | Manufacturing method of colloidal probe for atomic-force microscope |
| CN105628466A (en) * | 2015-12-24 | 2016-06-01 | 北京农业信息技术研究中心 | Corn stalk Micro-CT scanning sample and preparing method and application thereof |
-
2008
- 2008-04-17 CN CNA2008100361625A patent/CN101256133A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2481590C2 (en) * | 2010-08-17 | 2013-05-10 | Закрытое Акционерное Общество "Нанотехнология Мдт" | Manufacturing method of colloidal probe for atomic-force microscope |
| CN103018492A (en) * | 2012-11-21 | 2013-04-03 | 西安建筑科技大学 | Device and method for preparing PVDF (polyvinylidene fluoride) micro-particle probe by physical adhesion method |
| CN103018493A (en) * | 2012-11-21 | 2013-04-03 | 西安建筑科技大学 | Device and method for preparing PVDF (polyvinylidene fluoride) microparticle probe by using melting-sintering method |
| CN103018492B (en) * | 2012-11-21 | 2015-04-22 | 西安建筑科技大学 | Device and method for preparing PVDF (polyvinylidene fluoride) micro-particle probe by physical adhesion method |
| CN103018493B (en) * | 2012-11-21 | 2015-05-27 | 西安建筑科技大学 | Device and method for preparing PVDF (polyvinylidene fluoride) microparticle probe by using melting-sintering method |
| CN105628466A (en) * | 2015-12-24 | 2016-06-01 | 北京农业信息技术研究中心 | Corn stalk Micro-CT scanning sample and preparing method and application thereof |
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Open date: 20080903 |