CN104749399A - Preparation method and using device thereof for asphalt sample for AFM (Atomic Force Microscopy) observation - Google Patents
Preparation method and using device thereof for asphalt sample for AFM (Atomic Force Microscopy) observation Download PDFInfo
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Abstract
The invention discloses a preparation method for an asphalt sample for AFM (Atomic Force Microscopy) observation. The preparation method comprises the following steps of putting asphalt samples to be observed into a constant temperature oven and heating the asphalt samples to be observed to be melted; putting a clean sample holding vessel into an oven in the same temperature, taking out and putting the sample holding vessel on a horizontal table top, rapidly taking out the asphalt samples to be observed and evenly stirring, fetching appropriate asphalt samples to be observed to be injected into the sample holding vessel in one time, enabling the height of the asphalt samples to be slightly lower than the edge of the sample holding vessel, covering a cover and observing the sample holding vessel after the room temperature is cooled. The invention also discloses the sample holding vessel for the above method. The sample holding vessel comprises a vessel body (1) and a cover (2) which is matched with the vessel body (1); the cover (2) covers the vessel body (1). The preparation method is simple in operation and easy to operate, the asphalt samples form into smooth surfaces due to natural flow forming, shapes and thickness of the asphalt samples are effectively controlled through the size of the sample holding vessel, and AFM observation requirements for the flatness and the thickness of the samples are satisfied.
Description
Technical field
The invention belongs to pitch nanoscale microstructure and Senile Mouse technical field, relate to a kind of preparation method and equipment therefor thereof of the bitumen samples for atomic force microscope observation.
Background technology
Microstructure analysis is effective analytical technology of Asphalt Aging Study mechanism and Macro-Rheological Characterization energy, pavement performance, from common optical microscopy, electron microscope technique again to atom microtechnic, the application in pitch research has also had a lot of preliminary probing into.Wherein, what application was comparatively general has fluorescence microscopy (FM), scanning electron microscopy (SEM), atomic force microscopy (AFM) etc.Fluorescence microscopy is mainly used in Study Polymer Melts modified bitumen, and matrix pitch cannot reflect enough fluorescence and cannot apply, scanning electron microscope needs the operating environment of high vacuum, and sample needs gold-plated process, also cannot apply, and atomic force microscope (AFM) has high resolution (spatial resolution atom level 0.1nm), the surface topography (resolution of optical microscope is limited in 200 nanometers) of any types of materials can be measured on atom and molecular recognition rate, under any condition, shooting obtains matrix pitch, the nanostructured phase picture of modified bitumen, and power-distance Curve can be utilized to analyze the mechanical property of pitch nanoscale, as elastic modulus, hardness, dissipation energy, the performances such as adhesiveness quantize, it is harmless advanced microtechnic indispensable in the research of pitch nanoscale micromechanism phase.Therefore, compared with other Microbeam Analysis Techniques, AFM technology has unique advantage.
In recent years, atomic force microscopy was applied to asphalt material field by researcher gradually, and at present, one of maximum challenge is that observation sample is uneven, and flatness is not high.Seek a kind of simple and feasible preparation method to observe to make the bitumen samples of preparation be easy to AFM, being the basis that this technology is successfully applied to asphalt material microcosmic research field, is also matter of utmost importance urgently to be resolved hurrily.At present, common bitumen samples preparation method mainly contains solution spin-coating method, microslide heat drips method.
(1) solution spin-coating method:
First, under normal temperature by pitch by a certain percentage (10g:100ml) be dissolved in organic solvent triclene, toluene or other solvents and (carried out the thickness of Control Assay by the concentration of solution), obtain the mixed solution of asphalt solution; Then utilize spin coating instrument by solution coating on the glass sheet, finally sample is put into set baking oven or other vacuum equipments, vapor away remaining organic solvent, finally obtain comparatively level and smooth bitumen samples film.The sample flatness that this method for making sample obtains is relatively better, the thickness of asphalt membrane can be effectively controlled, but operate very complicated, the prices such as the testing equipment spin coating instrument needed are comparatively expensive, and organic solvent triclene, toluene are mostly extremely toxic substance, totally unfavorable to the health of experimenter, again, organic solvent itself and dosage size for the impact of pitch microscopic morphology structure, final conclusion not yet clear and definite at present.Therefore, this method should not be applied.
(2) microslide heat drips method:
It is liquid that asphalt sample to be measured is mainly heated to flowing by the method, then the pitch that takes a morsel drops in microslide middle position, and then microslide is placed in the baking oven of fixed temperature, bitumen samples flow dispersion is come formation thin film, then take out microslide sample, room temperature cooling is with to be observed.Obviously, this method is easy to operation, but problem be drip be coated with formed surface smoothness poor, be difficult to meet the flatness requirement of atomic force microscope for specimen surface, need again by microslide sample post bake to obtain level and smooth surface.Problem is: microslide film sample post bake, and bitumen samples is because the very little meeting of film thickness is aging rapidly, and the microscopic morphology structure of AFM observation truly can not reflect the Phase stracture of pitch; Add asphalt sample to flow arbitrarily on microslide, the film thickness finally formed and shape are difficult to effective control, should not carry out the comparison of parallel sample.Therefore, there is obvious weak point in the preparation method of above bitumen samples, is unfavorable for the application of atomic force microscopy in pitch Research of microstructure, is necessary to carry out improvement and standardization to preparation method of sample.
Summary of the invention
For the defect that the preparation method of existing bitumen samples exists, the object of this invention is to provide a kind of easy to operation, preparation method of preventing ageing of asphalt, effectively controlling the bitumen samples for atomic force microscope observation of asphalt membrane thickness and shape.
Another object of the present invention is to provide a kind of said method device used.
To achieve these goals, the present invention is by the following technical solutions:
The invention provides a kind of preparation method of the bitumen samples for atomic force microscope observation, comprise the following steps:
Asphalt sample to be observed is put into constant temperature oven, is heated to asphalt sample to be observed and all melts; The sample-containing dish of cleaning is put into the baking oven preheating of identical temperature, taking out sample-containing dish puts it on level table, rapid taking-up asphalt sample to be observed also stirs, get appropriate asphalt sample to be observed and once inject sample-containing dish immediately, height is a little less than sample-containing dish edge, cover block, observe after sample-containing dish at room temperature cools.
Described asphalt sample to be observed is matrix pitch or modified bitumen.
When described asphalt sample to be observed is matrix pitch, oven temperature is set as 130 DEG C.
When described asphalt sample to be observed is modified bitumen, oven temperature is set as 150 DEG C.
The time that described sample-containing dish puts into the baking oven preheating of identical temperature is at least 30min.
The time that described sample-containing dish at room temperature cools is at least 24h.
Present invention also offers the sample-containing dish that a kind of said method is used, comprise ware body and the block supporting with ware body, described block is placed on ware body.
Described ware body and block are all be made by metal.
Described metal is 304 stainless steels.
The shape of described ware body is cylindrical shape, comprises bottom surface and side.
The shape of described block is cylindrical shape, comprises upper bottom surface, side and is positioned at the block handle of upper bottom surface center upper portion position.
The diameter of described ware body bottom surface is 10mm, and the height of side is 2mm.
The present invention compared with the existing technology, has the following advantages and beneficial effect:
In method of the present invention testing sample only need heating once (first heated asphalt sample dose is large, short-term heating can not produce ageing of asphalt phenomenon), avoid the post bake of asphalt film, effectively prevent the catabiosis of pitch, the pitch phase observed can reflect pitch nanoscale Phase stracture really.
The pitch of flow state in method of the present invention, in metal sample-containing dish, natural flow is shaping, can effectively avoid the aging of asphalt film sample, can obtain good flatness, meet the observation requirements of atomic force microscope.
Due to the restriction of sample-containing dish size in method of the present invention, the thickness of bitumen samples and shape can be well controlled, so that the Comparison Study between parallel sample.
Method of the present invention sample-containing dish used is incidentally blocked a shot accordingly, effectively can prevent the pollution of specimen surface.
Method of the present invention is easy to operation, does not need the equipment of the costlinesses such as spin coating instrument.
Accompanying drawing explanation
Fig. 1 is the structural representation of ware body in the sample-containing dish of the embodiment of the present invention.
Fig. 2 is the structural representation of blocking a shot in the sample-containing dish of the embodiment of the present invention.
Fig. 3 is matrix pitch two-dimensional appearance image under an atomic force microscope.
Fig. 4 is SBS modified bitumen two-dimensional appearance image under an atomic force microscope.
Fig. 5 is two honeybee phases in matrix pitch two-dimensional appearance image.
Fig. 6 is the feature size quantization signifying figure of the honeybee phase of two shown in Fig. 5.
Wherein: 1 is ware body, 2 is block, and 3 is block handle.
Embodiment
Below in conjunction with accompanying drawing illustrated embodiment, the present invention is further detailed explanation.
Method of the present invention is all applicable for basis bitumen and modified bitumen.Embodiment mesostroma pitch is shell 70# matrix pitch, modified bitumen is SBS finished product asphaltum, atomic force microscope is the ICON model that German Brooker company produces, select PeakForce tapping mode of operation, according to the modulus properties of asphalt material own, select RTESPA model probe (f0=75kHz, k=3N/m), sweep limit is set as 20um*20um.
Embodiment 1
(1) 70# matrix pitch sample 200g to be observed is put into constant temperature oven, oven temperature sets 130 DEG C, is heated to pitch and all melts the liquid becoming flowing;
(2) the metal sample-containing dish (internal diameter 10mm, height 2mm) of cleaning is put into the baking oven of identical temperature, preheating 30min, in case produce bubble during bitumen samples moulding;
(3) metal sample-containing dish is taken out, and put it on level table, rapid taking-up asphalt sample also stirs, about 0.2g pitch is got with little spoon, once inject sample-containing dish immediately, highly a little less than sample-containing dish edge, as depicted in figs. 1 and 2, cover corresponding block, in case sample surfaces pollutes;
(4) sample-containing dish cools in room temperature, at least 24h, ensures that annealing process terminates, and pitch microscopic pattern returns to original state, with to be observed;
(5) according to microstructure image, quantitative analysis is carried out to the feature of structure peculiar in image.
Interpretation of result: Fig. 3 is matrix pitch two-dimensional appearance image under an atomic force microscope, from image, the honeybee phase structure that in shape appearance figure, stochastic distribution size differs, research is in the past verified, and two kinds of phases that honeybee phase structure is risen and fallen by light and dark, height form.Fig. 5 is two honeybee phases in matrix pitch two-dimensional appearance image, Fig. 6 is the feature size quantization signifying figure of the honeybee phase of two shown in Fig. 5, in Fig. 6, two honeybee phase morphologies distinctive in image are carried out to the extraction of height profile along honeybee phase long axis direction, in order to characterize honeybee phase structure characteristic dimension.From height profile curve map, although the length of honeybee phase structure is not of uniform size, but the quantized data extracted from contour curve, distance between honeybee phase structure light tone region and light tone region (dark areas and dark areas) is definite value, if d1 and d2 numerical value in Fig. 6 is at about 0.5um, just conform to the research of forefathers.
Embodiment 2
(1) SBS modified bitumen sample to be observed is put into constant temperature oven, the design temperature of oven temperature is 150 DEG C, and heated asphalt is to the liquid state that flows;
(2) the metal sample-containing dish (internal diameter 10mm, height 2mm) of cleaning is put into the baking oven of identical temperature, preheating 30min, in case produce bubble during bitumen samples moulding;
(3) take out metal sample-containing dish, and put it on level table, take out asphalt sample rapidly and stir, get about 0.2g pitch with little spoon and once inject sample-containing dish immediately, height, a little less than sample-containing dish edge, covers corresponding block, in case sample surfaces pollutes;
(4) sample-containing dish cools in room temperature, at least 24h, ensures that annealing process terminates, and pitch microscopic pattern returns to original state, with to be observed;
(5) according to microstructure image, quantitative analysis is carried out to the feature of structure peculiar in image.
Interpretation of result: Fig. 4 is SBS modified bitumen two-dimensional appearance image under an atomic force microscope, as can be seen from the figure, in SBS modified bitumen, also dispersion also exists honeybee phase structure, because adding of modifier causes the distribution of the height of nanoscale pitch pattern to there are some differences with matrix pitch, being embodied in shape appearance figure, is namely the difference of color in image.
Embodiment 3
The sample-containing dish that described in embodiment 1 and 2, method is used, as depicted in figs. 1 and 2, Fig. 1 is the structural representation of ware body in the sample-containing dish of the embodiment of the present invention; Fig. 2 is the structural representation of blocking a shot in the sample-containing dish of the embodiment of the present invention; Comprise ware body 1 and the block 2 supporting with ware body 1, described block 2 is placed on ware body 1, wherein: ware body 1 and block 2 are all be made by metal, and metal is stainless steel 304; The shape of ware body 1 is cylindrical shape, comprises bottom surface and side; The shape of block 2 is cylindrical shapes, comprises upper bottom surface, side and is positioned at the block handle 3 of upper bottom surface center upper portion position; The diameter of ware body 1 bottom surface is 10mm, and the height of side is 2mm.
Above-mentioned is can understand and apply the invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (10)
1., for a preparation method for the bitumen samples of atomic force microscope observation, it is characterized in that: comprise the following steps:
Asphalt sample to be observed is put into constant temperature oven, is heated to asphalt sample to be observed and all melts; The sample-containing dish of cleaning is put into the baking oven preheating of identical temperature, taking out sample-containing dish puts it on level table, rapid taking-up asphalt sample to be observed also stirs, get appropriate asphalt sample to be observed and once inject sample-containing dish immediately, height is a little less than sample-containing dish edge, cover block, observe after sample-containing dish at room temperature cools.
2. the preparation method of the bitumen samples for atomic force microscope observation according to claim 1, is characterized in that: described asphalt sample to be observed is matrix pitch or modified bitumen.
3. the preparation method of the bitumen samples for atomic force microscope observation according to claim 2, is characterized in that: when described asphalt sample to be observed is matrix pitch, oven temperature is set as 130 DEG C.
4. the preparation method of the bitumen samples for atomic force microscope observation according to claim 2, is characterized in that: when described asphalt sample to be observed is modified bitumen, oven temperature is set as 150 DEG C.
5. the preparation method of the bitumen samples for atomic force microscope observation according to claim 1, is characterized in that: the time that described sample-containing dish puts into the baking oven preheating of identical temperature is at least 30min.
6. the preparation method of the bitumen samples for atomic force microscope observation according to claim 1, is characterized in that: the time that described sample-containing dish at room temperature cools is at least 24h.
7. the sample-containing dish that the arbitrary described method of claim 1 to 6 is used, it is characterized in that: comprise ware body (1) and the block (2) supporting with ware body (1), described block (2) is placed on ware body (1).
8. sample-containing dish according to claim 7, is characterized in that: described ware body (1) and block (2) are all be made by metal;
The shape of described ware body (1) is cylindrical shape further, comprises bottom surface and side;
The shape of described block (2) is cylindrical shape further, comprises upper bottom surface, side and is positioned at the block handle (3) of upper bottom surface center upper portion position.
9. sample-containing dish according to claim 8, is characterized in that: described metal is 304 stainless steels.
10. sample-containing dish according to claim 8, is characterized in that: the diameter of described ware body (1) bottom surface is 10mm, and the height of side is 2mm.
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| CN106248998A (en) * | 2016-07-22 | 2016-12-21 | 同济大学 | A kind of asphalt Research on Mechanical Properties method based on atomic force microscopy |
| CN106405158A (en) * | 2016-11-15 | 2017-02-15 | 广州肖宁道路工程技术研究事务所有限公司 | Sample preparation device and method suitable for atomic force microscope |
| CN106443076A (en) * | 2016-09-20 | 2017-02-22 | 李波 | Asphalt sample preparation device and method suitable for atomic force microscopy testing |
| CN107037239A (en) * | 2016-11-28 | 2017-08-11 | 内蒙古工业大学 | The essence control thermoforming preparation method of bitumen samples is observed suitable for AFM |
| CN110186811A (en) * | 2019-07-01 | 2019-08-30 | 哈尔滨工业大学 | A kind of pitch Micro dynamic rheological characteristic test method |
| CN110208192A (en) * | 2019-06-28 | 2019-09-06 | 中国计量大学 | A kind of planchet holding meat products and the application at source tracing to the source |
| 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 |
| CN111855565A (en) * | 2020-07-21 | 2020-10-30 | 南京林业大学 | Method for testing effective mixing amount of direct-vat-set high-viscosity asphalt modifier |
| CN114353706A (en) * | 2022-01-11 | 2022-04-15 | 哈尔滨工业大学 | Asphalt two-dimensional morphology determination method based on environmental scanning electron microscope |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106248998A (en) * | 2016-07-22 | 2016-12-21 | 同济大学 | A kind of asphalt Research on Mechanical Properties method based on atomic force microscopy |
| CN106443076A (en) * | 2016-09-20 | 2017-02-22 | 李波 | Asphalt sample preparation device and method suitable for atomic force microscopy testing |
| CN106405158A (en) * | 2016-11-15 | 2017-02-15 | 广州肖宁道路工程技术研究事务所有限公司 | Sample preparation device and method suitable for atomic force microscope |
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| CN110208192A (en) * | 2019-06-28 | 2019-09-06 | 中国计量大学 | A kind of planchet holding meat products and the application at source tracing to the source |
| CN110186811A (en) * | 2019-07-01 | 2019-08-30 | 哈尔滨工业大学 | A kind of pitch Micro dynamic rheological characteristic test method |
| CN110186811B (en) * | 2019-07-01 | 2021-06-25 | 哈尔滨工业大学 | Method for testing microcosmic dynamic rheological property of asphalt |
| 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 |
| CN111855565A (en) * | 2020-07-21 | 2020-10-30 | 南京林业大学 | Method for testing effective mixing amount of direct-vat-set high-viscosity asphalt modifier |
| CN114353706A (en) * | 2022-01-11 | 2022-04-15 | 哈尔滨工业大学 | Asphalt two-dimensional morphology determination method based on environmental scanning electron microscope |
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Application publication date: 20150701 |