CN106405158A - Sample preparation device and method suitable for atomic force microscope - Google Patents
Sample preparation device and method suitable for atomic force microscope Download PDFInfo
- Publication number
- CN106405158A CN106405158A CN201611003504.4A CN201611003504A CN106405158A CN 106405158 A CN106405158 A CN 106405158A CN 201611003504 A CN201611003504 A CN 201611003504A CN 106405158 A CN106405158 A CN 106405158A
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- sample
- storage device
- pitch
- sample preparation
- sample storage
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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]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/20—Sample handling devices or methods
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Radiology & Medical Imaging (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a sample preparation device and method suitable for an atomic force microscope. The device comprises a substrate and a sample storage device. The substrate is arranged under the sample storage device which is arranged on the substrate. The sample storage device is a hollow cylinder whose side heights are the same. The substrate and the sample storage device are mutually connected through the adhesion of asphalt transferred to the sample storage device. By using the device, the film thickness of all samples can be consistent, the influence of the film thickness on a test result is eliminated, and the smooth surface of a sample is ensured.
Description
Technical field
The present invention relates to AFM sample preparation technology field, more particularly to one kind is applied to atomic force microscopy
The sample preparation apparatus of mirror and method.
Background technology
Pitch as a kind of widely used petrochemicals, furtherd investigate, but is subject to by its macro property
It is limited to the application of science and technology, its microcosmic effect mechanism is fully explained not yet.AFM can be examined as one kind
Measure sample surfaces Nano grade pattern and the instrument of mechanical characteristic has been widely applied in each research field, study at present
Personnel are just attempting to atomic force microscope observation pitch microscopic appearance and by the active force detection drip between probe and sample
Blue or green micromechanics, thus studying pitch microcosmic effect mechanism and setting up the connection between pitch microscopic characteristics and macro property
System.
The preparation of sample is to carry out the important step before asphalt test by AFM, and the quality of sample preparation is determined
Determine accuracy and the reliability of testing result, the method for current atom force microscope asphalt sample preparation mainly has solution spraying method
With heating sessile drop method.Solution spraying method utilizes solvent to dissolve pitch, can destroy the original structure of pitch it is impossible to truly reflect pitch
Microscopic property, and organic solvent toxicity used is stronger, and solution spraying method preparation facilities complexity is loaded down with trivial details simultaneously.Heating sessile drop method
Uncontrollable sample thickness, leads to assay reproducibility poor.The preparation facilities of solution spraying method and heating sessile drop method simultaneously
Prepared pitch can be led to lepthymenia and produce substrate effect, the accuracy of impact result of the test.
Content of the invention
It is an object of the invention to provide a kind of sample preparation apparatus being applied to AFM and method, by sample
Storage device is controlled to sample thickness and makes sample surfaces smooth.
For achieving the above object, the invention provides following scheme：
A kind of sample preparation apparatus being applied to AFM, including substrate, sample storage device；Described substrate sets
Put under described sample storage device, described sample storage device is placed in described substrate, described sample storage device is hollow
Cylinder, described hollow cylinder profile height is identical, and described substrate and described sample storage device rely on and be transferred to described sample
Asphalt adhesion in product storage device is connected with each other.
Optionally, also include：Sample transfer device；
Described sample transfer device includes sample adsorption part, support section and handle portion；Described sample transfer device
Material is stainless steel material；
Described sample support part is cylinder, and described sample adsorption part is cone, is used for preventing a transfer amount
Excessively；
Described handle portion is in 90 ° with described support section, for facilitating the operation of transfer device.
Optionally, described substrate is 20mm × 20mm mica sheet or cover glass；
The high 1.5mm of described sample storage device, internal diameter is 8mm, and external diameter is 10mm, and described sample storage device material is not
Rust Steel material.
Optionally, described sample adsorption partly long 5mm；
Described support section a diameter of 1mm, long 100mm；
The long 15mm of described handle portion.
A kind of sample preparation methods being applied to AFM, methods described is applied to above-mentioned sample preparation apparatus,
Methods described comprises the steps：
Described pitch is heated, makes described pitch be in flowable state；
Described sample storage device is positioned on described substrate；
Described pitch in flowable state is transferred to sample storage device, described substrate is relied on described sample storage device
The adhesiveness of described pitch is bonding；
Described sample preparation apparatus are carried out be heated to described asphalt surface smooth；
Cooling sample simultaneously puts into drying box；
Annealing more than 24h, obtains final AFM asphalt sample.
Optionally, described described pitch is heated：
Described pitch is put in described baking oven, oven temperature is adjusted according to pitch species, keeping temperature 2-3h, up to institute
Stating pitch is in flowable state.
Optionally, described the described pitch in flowable state is transferred to sample storage device, also include：
The described described pitch in flowable state is highly flushed with described sample storage device.
The specific embodiment being provided according to the present invention, the invention discloses following technique effect：
The present invention passes through to prepare asphalt sample using substrate, sample storage device, can be controlled by sample storage device
All samples thickness is identical, thus eliminating the test error brought because of thickness difference, avoiding simultaneously and being produced because sample is excessively thin
Raw substrate effect, improves the confidence level of result of the test.Meanwhile, sample storage device profile height is identical ensures that sample is put down
Whole, decrease because affecting produced by sample surfaces out-of-flatness.This sample preparation apparatus structure is simple and improves atomic force and shows
The accuracy that micro mirror detects to asphalt sample.
Brief description
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to institute in embodiment
Need use accompanying drawing be briefly described it should be apparent that, drawings in the following description be only the present invention some enforcement
Example, for those of ordinary skill in the art, without having to pay creative labor, can also be according to these accompanying drawings
Obtain other accompanying drawings.
Fig. 1 is substrate schematic diagram in the embodiment of the present invention；
Fig. 2 is sample storage device schematic diagram in the embodiment of the present invention；
Fig. 3 is sample transfer device schematic diagram in the embodiment of the present invention；
Fig. 4 is sample preparation apparatus schematic diagram in the embodiment of the present invention；
Fig. 5 is sample preparation methods flow chart in the embodiment of the present invention；
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation description is it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of not making creative work
Embodiment, broadly falls into the scope of protection of the invention.
It is an object of the invention to provide a kind of sample preparation apparatus being applied to AFM and method.
Understandable for enabling the above objects, features and advantages of the present invention to become apparent from, below in conjunction with the accompanying drawings and specifically real
The present invention is further detailed explanation to apply mode.
Fig. 4 is sample preparation apparatus schematic diagram in the embodiment of the present invention；
Referring to Fig. 4, this device includes：Including substrate 101, sample storage device 201；Described substrate 101 is arranged on described
Under sample storage device 201, described sample storage device 201 is placed in described substrate 101, and described sample storage device 201 is
Hollow cylinder, described hollow cylinder profile height is identical, and described substrate 101 and described sample storage device 201 rely on and turn
Pitch 401 adhesiveness moving in described sample storage device 201 is connected with each other.Optionally, also include：Sample transfer device
301；
Described sample transfer device 301 includes sample adsorption part 302, support section 303 and handle portion 304；Described
Sample transfer device 301 material is stainless steel material；
Described sample adsorption part 302 is cone, for adsorbing described pitch 401, prevents a transfer amount excessive；
Described handle portion 304 is in 90 ° with described support section 303, for controlling the absorption of described pitch 401.
Optionally, described substrate 101 is mica sheet or the cover glass of 20mm × 20mm；
The high 1.5mm of described sample storage device 201, internal diameter is 8mm, and external diameter is 10mm, described sample storage device 201 material
Matter is stainless steel material.
Optionally, the long 5mm of described sample adsorption part 302；
Described support section 303 a diameter of 1mm, long 100mm；
The long 15mm of described handle portion 304.
Fig. 5 is sample preparation methods flow chart in the embodiment of the present invention.
Referring to Fig. 5, a kind of sample preparation methods being applied to AFM, methods described is applied to above-mentioned sample system
Standby device, methods described comprises the steps：
Step 501：Heating makes pitch be in flowable state；Described pitch is heated, makes described pitch be in flowable state, will fill
The beaker having pitch is put in baking oven, and adjusts oven temperature (for example for 30# matrix according to specification according to different pitches species
Pitch, oven temperature is adjusted to 160 DEG C), keep oven temperature 2～3h until pitch is in flowable state.
Step 502：Described sample storage device is positioned on described substrate；
Step 503：Described pitch in flowable state is transferred to sample storage device, described substrate and described sample storage
Device relies on the adhesiveness of described pitch bonding.Pitch instilling in substrate in a small amount of beaker is adsorbed using sample transfer device
Sample storage device in highly flush with sample storage device until asphalt sample, substrate and sample storage device dependence pitch
Adhesiveness bonding.
Step 504：Described sample preparation apparatus are carried out be heated to described asphalt surface smooth；Because pitch is in room
Temperature is lower to be cooled down rapidly, and viscosity larger it is impossible to formation flat surface, therefore sample preparation apparatus continue to put into 10min in baking oven
Left and right is completely smooth smooth up to asphalt sample surface.
Step 505：Cooling sample simultaneously puts into drying box.It is removed and placed in culture dish in baking oven after sample surfaces are smooth
In be cooled to room temperature, and by culture dish put in drying box with prevent sample surfaces be subject to dust in air pollution and prevent sky
Water adsorption in gas leads to testing result inaccurate in sample surfaces etc..
Step 506：Annealing more than 24h, obtains final AFM asphalt sample.
Step 507：Device is carried out, dries to reuse.After sample after AFM detection, if
It is no longer necessary to preservation sample it can be cleaned, dry in case reusing using kerosene etc..
In this specification, each embodiment is described by the way of going forward one by one, and what each embodiment stressed is and other
The difference of embodiment, between each embodiment identical similar portion mutually referring to.
Specific case used herein is set forth to the principle of the present invention and embodiment, the saying of above example
Bright it is only intended to help and understands the method for the present invention and its core concept；Simultaneously for one of ordinary skill in the art, foundation
The thought of the present invention, all will change in specific embodiments and applications.In sum, this specification content is not
It is interpreted as limitation of the present invention.
Claims (8)
1. it is characterised in that including substrate, samples storage fills a kind of sample preparation apparatus being applied to AFM
Put；Described substrate is arranged under described sample storage device, and described sample storage device is placed in described substrate, and described sample is deposited
Saving is set to hollow cylinder, and described hollow cylinder profile height is identical, and described substrate and described sample storage device rely on
The asphalt adhesion being transferred in described sample storage device is connected with each other.
2. sample preparation apparatus according to claim 1 are it is characterised in that also include：Sample transfer device；
Described sample transfer device includes sample adsorption part, support section and handle portion；Described sample transfer device material
For stainless steel material；
Described support section is cylinder, and described sample adsorption part is cone, is used for preventing a transfer amount excessive；
Described handle portion is partly in 90 ° with described support section, is used for facilitating transition of operation device.
3. sample preparation apparatus according to claim 1 are it is characterised in that also include：
Described substrate is 20mm × 20mm mica sheet or cover glass；
The a height of 1.5mm of described sample storage device, internal diameter is 8mm, and external diameter is 10mm, and described sample storage device material is stainless
Steel material.
4. sample preparation apparatus according to claim 2 it is characterised in that：
Described sample adsorption partly long 5mm；
Described support section a diameter of 1mm, long 100mm；
The long 15mm of described handle portion.
5. a kind of sample preparation methods being applied to AFM are it is characterised in that methods described is applied to claim 1
To the sample preparation apparatus described in claim 4, methods described comprises the steps：
Described pitch is heated, makes described pitch be in flowable state；
Described sample storage device is positioned on described substrate；
Described pitch in flowable state is transferred to sample storage device, described substrate and described sample storage device rely on described
The adhesiveness of pitch is bonding；
Described sample preparation apparatus are carried out be heated to described asphalt surface smooth；
Cool down described sample preparation apparatus and put into drying box；
Annealing more than 24h, obtains final AFM asphalt sample.
6. sample preparation methods according to claim 5 are it is characterised in that described heat to described pitch：
Described pitch is put in described baking oven, oven temperature is adjusted according to pitch species, keeping temperature 2-3h is up to described drip
Blue or green is in flowable state.
7. sample preparation methods according to claim 5 are it is characterised in that described shift the described pitch in flowable state
To sample storage device, also include：
The described described pitch in flowable state is highly flushed with described sample storage device.
8. sample preparation methods according to claim 5 are it is characterised in that described sample preparation apparatus of described cooling putting
Enter drying box, also include：
It is removed and placed in being cooled to room temperature after described asphalt surface is smooth in described baking oven culture dish.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611003504.4A CN106405158A (en) | 2016-11-15 | 2016-11-15 | Sample preparation device and method suitable for atomic force microscope |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611003504.4A CN106405158A (en) | 2016-11-15 | 2016-11-15 | Sample preparation device and method suitable for atomic force microscope |
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| Publication Number | Publication Date |
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| CN106405158A true CN106405158A (en) | 2017-02-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201611003504.4A Pending CN106405158A (en) | 2016-11-15 | 2016-11-15 | Sample preparation device and method suitable for atomic force microscope |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956261A (en) * | 2018-09-07 | 2018-12-07 | 香港理工大学 | A kind of preparation method of asphalt film |
| CN110850115A (en) * | 2019-10-18 | 2020-02-28 | 东南大学 | Preparation device and method suitable for atomic force microscope thermal regeneration asphalt sample |
| CN113433347A (en) * | 2021-06-24 | 2021-09-24 | 中国科学院青海盐湖研究所 | AFM sample for hydrous salt phase change energy storage material and preparation method and application thereof |
Citations (4)
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| CN1260737A (en) * | 1997-06-17 | 2000-07-19 | 康宁股份有限公司 | System and mfg. of small volume transferer |
| CN104749399A (en) * | 2015-03-24 | 2015-07-01 | 同济大学 | Preparation method and using device thereof for asphalt sample for AFM (Atomic Force Microscopy) observation |
| CN104897451A (en) * | 2015-06-26 | 2015-09-09 | 山东钢铁股份有限公司 | Asphalt softening point test sample preparation device |
| CN206177989U (en) * | 2016-11-15 | 2017-05-17 | 广州肖宁道路工程技术研究事务所有限公司 | Sample preparation device suitable for atomic force microscope |
-
2016
- 2016-11-15 CN CN201611003504.4A patent/CN106405158A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1260737A (en) * | 1997-06-17 | 2000-07-19 | 康宁股份有限公司 | System and mfg. of small volume transferer |
| CN104749399A (en) * | 2015-03-24 | 2015-07-01 | 同济大学 | Preparation method and using device thereof for asphalt sample for AFM (Atomic Force Microscopy) observation |
| CN104897451A (en) * | 2015-06-26 | 2015-09-09 | 山东钢铁股份有限公司 | Asphalt softening point test sample preparation device |
| CN206177989U (en) * | 2016-11-15 | 2017-05-17 | 广州肖宁道路工程技术研究事务所有限公司 | Sample preparation device suitable for atomic force microscope |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956261A (en) * | 2018-09-07 | 2018-12-07 | 香港理工大学 | A kind of preparation method of asphalt film |
| CN110850115A (en) * | 2019-10-18 | 2020-02-28 | 东南大学 | Preparation device and method suitable for atomic force microscope thermal regeneration asphalt sample |
| CN113433347A (en) * | 2021-06-24 | 2021-09-24 | 中国科学院青海盐湖研究所 | AFM sample for hydrous salt phase change energy storage material and preparation method and application thereof |
| CN113433347B (en) * | 2021-06-24 | 2022-11-08 | 中国科学院青海盐湖研究所 | AFM sample for hydrous salt phase change energy storage material and preparation method and application thereof |
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