CN103901231A - Preparation method for asphalt sample suitable for atomic force microscope observation - Google Patents
Preparation method for asphalt sample suitable for atomic force microscope observation Download PDFInfo
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- CN103901231A CN103901231A CN201410138670.XA CN201410138670A CN103901231A CN 103901231 A CN103901231 A CN 103901231A CN 201410138670 A CN201410138670 A CN 201410138670A CN 103901231 A CN103901231 A CN 103901231A
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Abstract
The invention discloses a preparation method for an asphalt sample suitable for atomic force microscope observation. The preparation method includes the steps that solid asphalt is dissolved in organic solvent at normal temperature to prepare asphalt solution, and the mass volume ratio of the asphalt and the organic solvent in the asphalt solution is 5 g-15g: 100 ml; a glass slide is placed on the plane or fixed to the center of a centrifugal machine, and the centrifugal machine is started at the rotation speed smaller than or equal to 5000 rpm; the asphalt solution is dripped on the glass slide, and the glass slide is placed on the plane to stand for 5-10 minutes; the glass slide is fixed to the center of the centrifugal machine for centrifuge by 5 minutes -10 minutes; the glass slide is placed into a drying box at the temperature of 50 DEG C-70 DEG C for 15 minutes-20 minutes, then taken out and observed; meanwhile, the thickness of an asphalt film can be controlled through the method, and possibility is provided for researching influences on asphalt micro-phase separation behaviors by changes of the thickness of the film.
Description
Technical field
The present invention relates to pitch Study on Microstructure field, relate in particular to the pitch preparation method of sample that is applicable to atomic force microscope observation.
Background technology
Atomic force microscope can observe the micromechanism of several nanometers of material surface to hundreds of micro-meter scale, can be used for high precision and the high sensitivity quantitation analysis of surface microroughness, contributes to researcher to be familiar with in all directions the structure-performance relation of material.
In recent years, utilize the research of atomic force microscope research pitch micromechanism phase separation to get the attention, and the top priority that correlation test is carried out is the pitch sample that preparation is applicable to observation.
At present, the most frequently used method for making sample is hot tapping technique, and main preparation flow is as follows:
(1) asphalt heating is extremely liquid; Matrix pitch is heated to 120 ℃; Modified bitumen is heated to 160 ℃;
(2) a small amount of pitch is dropped in to microslide central authorities;
(3) microslide is placed in to baking oven (150 ℃) about 10min so that pitch is shattered into the diaphragm of diameter 1cm left and right;
(4) sample is taken out and naturally cools to room temperature, use to be observed.
Use the method to prepare pitch sample simple and efficient, but have following two problems:
(1) in sample preparation process, need repeatedly to heat, easily make ageing of asphalt, affect observed result.
(2) existing research points out that pitch can be divided into two-phase according to spinodal decomposition mechanism under micro-scale, and one of important content of research pitch phase separation is exactly to study the impact of thickness on pitch microcosmic phase.Even if but due to pitch also thickness comparatively under hot conditions, therefore the conventional method of pass through Centrifugal Machine Control film thickness (the higher film of centrifuge speed is thinner) is also inapplicable at this.
By above analysis, correlative study is needed a kind of new pitch preparation method of sample badly to overcome above-mentioned 2 deficiencies.
Summary of the invention
The object of this invention is to provide one and be applicable to atomic force microscope observation pitch preparation method of sample, easily aging in preparation process to solve prior art medium pitch sample, the uppity defect of film thickness.
For addressing the above problem, the present invention by the following technical solutions:
One is applicable to atomic force microscope observation pitch preparation method of sample, comprises the steps:
Under step 1, normal temperature, solid bitumen is dissolved in organic solvent and is mixed with cold primer-oil, described cold primer-oil medium pitch and organic solvent mass volume ratio are 5～15g:100ml;
Step 2, microslide be placed on to plane or be fixed on hydro-extractor central authorities, starting hydro-extractor, rotating speed≤5000rpm;
Step 3, cold primer-oil described in step 1 is dripped on microslide described in step 2, microslide is placed the 5～10min that leaves standstill in the plane; Microslide is fixed on the centrifugal 5～10min of hydro-extractor central authorities;
Step 4, the microslide that step 3 is obtained are put into 50～70 ℃ of baking oven 15～20min, take out afterwards, observe.
Described in step 1, organic solvent is triclene, toluene or cyclohexane.
Described in step 2, microslide is fixed on hydro-extractor central authorities with adhesive tape.
Step 3 cold primer-oil drips 3～5 on microslide.
Beneficial effect of the present invention:
Method provided by the invention can farthest reduce the impact of pitch sample preparation process heat aging factor on pitch micromechanism; The method can realize the control of asphalt membrane thickness simultaneously, for the variation of research thickness provides possibility to the impact of pitch micron-scale phase separation behavior.
Accompanying drawing explanation
Fig. 1 is the pitch sample for atomic force microscope observation prepared by embodiment 1.
Fig. 2 is the pitch micron-scale phase separation behavior that the pitch sample for atomic force microscope observation prepared by embodiment 1 utilizes atomic force microscope observation.
Fig. 3 is the pitch micron-scale phase separation behavior that pitch sample prepared by background technology hot tapping technique utilizes atomic force microscope observation.
Fig. 4 is the pitch micromechanism that the pitch sample for atomic force microscope observation prepared by embodiment 1 utilizes atomic force microscope observation.
Fig. 5 is the pitch sample for atomic force microscope observation prepared by embodiment 2.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is done further and explained.Following embodiment does not limit the present invention in any form, and all employings are equal to replaces or technical scheme that the mode of equivalent transformation obtains, all among protection scope of the present invention.
One is applicable to atomic force microscope observation pitch preparation method of sample, comprises the steps:
Under step 1, normal temperature, solid bitumen is dissolved in triclene, toluene or cyclohexane and is mixed with cold primer-oil, described cold primer-oil medium pitch and organic solvent mass volume ratio are 5～15g:100ml;
Step 2, microslide placed in the plane or be fixed on hydro-extractor central authorities with adhesive tape, starting hydro-extractor, rotating speed≤5000rpm;
Step 3, draw cold primer-oil described in 3～5 step 1 drip on microslide described in step 2 with suction pipe, microslide is placed standing 5～10min in the plane; Microslide is fixed on the centrifugal 5～10min of hydro-extractor central authorities; Change the change of controlling diaphragm thickness by the rotating speed of hydro-extractor, the higher film of centrifuge speed is thinner;
Step 4, the microslide that step 3 is obtained are put into 50～70 ℃ of baking oven 15～20min, make the annealing of pitch sample realize the recovery of pitch micromechanism, take out afterwards, observe.
The inventive method is applicable to all pitch, comprises basis bitumen and modified bitumen.No. 50 matrix pitches that the solid bitumen that following examples are used provides for Jiangyin Bao Li pitch incorporated company.The microslide specification that following examples are used is 76mm*26mm.
1, in beaker, pour 10ml triclene into, and cut 1g solid bitumen with blade and put into wherein, pitch dissolves be mixed with cold primer-oil completely.
2, microslide is placed in horizontal table top.
3, draw 3～5 cold primer-oils with suction pipe and drip on microslide, leave standstill 5min.
4, microslide is put into 60 ℃ of baking oven 20min, taken out afterwards and obtain being applicable to atomic force microscope observation pitch sample.
Fig. 1 is the pitch sample for atomic force microscope observation prepared by the present embodiment, does not use rotating speed in preparation process, i.e. the thickest asphalt membrane of thickness in theory.
The pitch sample of preparation is utilized to the pitch micron-scale phase separation behavior of atomic force microscope observation, as shown in Figure 2, having the structure that black and white strip is alternate is crystal phase, and amorphous phase around distributes.Fig. 3 is the pitch micron-scale phase separation behavior that pitch sample prepared by background technology hot tapping technique (pitch of use is identical with the present embodiment) utilizes atomic force microscope observation.The micromechanism size, the distribution that in Fig. 2, observe are comparatively even, and the microstructure sizes observing in Fig. 3 is larger, and difference of them is obvious, and supposition is because the impact of the aging action that different thickness and heating cause.
Fig. 4 is the pitch micromechanism of atomic force microscope observation, can find out that crystallization phase owing to presenting typical sinusoidal form under surface stress effect, and crest place is corresponding to white stripes in Fig. 2, and trough place is corresponding to blackstreak in Fig. 2.
Embodiment 2
1, in beaker, pour 10ml triclene into, and cut 1g solid bitumen with blade and put into wherein, pitch dissolves be mixed with cold primer-oil completely.
2, microslide is fixed on to hydro-extractor central authorities with adhesive tape, starts hydro-extractor, rotating speed is 333rpm.
3, draw 3～5 cold primer-oils with suction pipe and drip on microslide, centrifugal 5min.
4, microslide is put into 60 ℃ of baking oven 20min, taken out afterwards and obtain being applicable to atomic force microscope observation pitch sample.Fig. 5 is the pitch sample for atomic force microscope observation prepared by the present embodiment.
Embodiment 3
1, in beaker, pour 10ml toluene into, and cut 0.5g solid bitumen with blade and put into wherein, pitch dissolves be mixed with cold primer-oil completely.
2, microslide is fixed on to hydro-extractor central authorities with adhesive tape, starts hydro-extractor, rotating speed is 2500rpm.
3, draw 3～5 cold primer-oils with suction pipe and drip on microslide, centrifugal 5min.
4, microslide is put into 50 ℃ of baking oven 20min, taken out afterwards and obtain being applicable to atomic force microscope observation pitch sample.
Embodiment 4
1, in beaker, pour 10ml cyclohexane into, and cut 1.5g solid bitumen with blade and put into wherein, pitch dissolves be mixed with cold primer-oil completely.
2, microslide is fixed on to hydro-extractor central authorities with adhesive tape, starts hydro-extractor, rotating speed is 5000rpm.
3, draw 3～5 cold primer-oils with suction pipe and drip on microslide, centrifugal 10min.
4, microslide is put into 70 ℃ of baking oven 10min, taken out afterwards and obtain being applicable to atomic force microscope observation pitch sample.
Claims (4)
1. be applicable to an atomic force microscope observation pitch preparation method of sample, it is characterized in that, comprise the steps:
Under step 1, normal temperature, solid bitumen is dissolved in organic solvent and is mixed with cold primer-oil, described cold primer-oil medium pitch and organic solvent mass volume ratio are 5～15g:100ml;
Step 2, microslide placed in the plane or is fixed on hydro-extractor central authorities, starting hydro-extractor, rotating speed≤5000rpm;
Step 3, cold primer-oil described in step 1 is dripped on microslide described in step 2, microslide is placed the 5～10min that leaves standstill in the plane; Microslide is fixed on the centrifugal 5～10min of hydro-extractor central authorities;
Step 4, the microslide that step 3 is obtained are put into 50～70 ℃ of baking oven 15～20min, take out afterwards, observe.
2. the atomic force microscope observation pitch preparation method of sample that is applicable to according to claim 1, is characterized in that, organic solvent is triclene, toluene or cyclohexane described in step 1.
3. the atomic force microscope observation pitch preparation method of sample that is applicable to according to claim 1 and 2, is characterized in that, microslide is fixed on hydro-extractor central authorities with adhesive tape described in step 2.
4. the atomic force microscope observation pitch preparation method of sample that is applicable to according to claim 1 and 2, is characterized in that, step 3 cold primer-oil drips 3～5 on microslide.
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| CN201410138670.XA CN103901231A (en) | 2014-04-08 | 2014-04-08 | Preparation method for asphalt sample suitable for atomic force microscope observation |
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| CN201410138670.XA CN103901231A (en) | 2014-04-08 | 2014-04-08 | Preparation method for asphalt sample suitable for atomic force microscope observation |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN106769277A (en) * | 2016-11-15 | 2017-05-31 | 广州肖宁道路工程技术研究事务所有限公司 | A kind of method and system for obtaining pitch microcosmic surface distributed intelligence |
| CN110208578A (en) * | 2019-06-24 | 2019-09-06 | 河海大学 | A kind of adhesive property evaluation method of foam warm-mixed asphalt difference foaming stages |
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| US5654546A (en) * | 1995-11-07 | 1997-08-05 | Molecular Imaging Corporation | Variable temperature scanning probe microscope based on a peltier device |
| CN101324528A (en) * | 2008-07-16 | 2008-12-17 | 清华大学 | Thin film with local field enhancement function and preparing method thereof |
| JP2012063319A (en) * | 2010-09-17 | 2012-03-29 | Toppan Printing Co Ltd | Atomic force microscope observation method of polymeric material at high temperature state |
| CN202204831U (en) * | 2011-02-01 | 2012-04-25 | 国家纳米科学中心 | Substrate applicable to suspension state cell atomic force microscope eutopic imaging |
| CN103529244A (en) * | 2013-10-28 | 2014-01-22 | 东南大学 | Method based on atomic force microscope for researching microscopic characteristics of asphalt |
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2014
- 2014-04-08 CN CN201410138670.XA patent/CN103901231A/en active Pending
Patent Citations (5)
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| US5654546A (en) * | 1995-11-07 | 1997-08-05 | Molecular Imaging Corporation | Variable temperature scanning probe microscope based on a peltier device |
| CN101324528A (en) * | 2008-07-16 | 2008-12-17 | 清华大学 | Thin film with local field enhancement function and preparing method thereof |
| JP2012063319A (en) * | 2010-09-17 | 2012-03-29 | Toppan Printing Co Ltd | Atomic force microscope observation method of polymeric material at high temperature state |
| CN202204831U (en) * | 2011-02-01 | 2012-04-25 | 国家纳米科学中心 | Substrate applicable to suspension state cell atomic force microscope eutopic imaging |
| CN103529244A (en) * | 2013-10-28 | 2014-01-22 | 东南大学 | Method based on atomic force microscope for researching microscopic characteristics of asphalt |
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| PAULI等: ""Morphology of asphalts, asphalt fractions and model wx-doped asphalts studied by atomic force microscopy"", 《INTERNATIONAL JOURNAL OF PAVEMENT ENGINEERING》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN106769277A (en) * | 2016-11-15 | 2017-05-31 | 广州肖宁道路工程技术研究事务所有限公司 | A kind of method and system for obtaining pitch microcosmic surface distributed intelligence |
| CN110208578A (en) * | 2019-06-24 | 2019-09-06 | 河海大学 | A kind of adhesive property evaluation method of foam warm-mixed asphalt difference foaming stages |
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