CN109900930A - A kind of asphalt modification effect evaluation method based on atomic force microscope - Google Patents
A kind of asphalt modification effect evaluation method based on atomic force microscope Download PDFInfo
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- CN109900930A CN109900930A CN201910160755.0A CN201910160755A CN109900930A CN 109900930 A CN109900930 A CN 109900930A CN 201910160755 A CN201910160755 A CN 201910160755A CN 109900930 A CN109900930 A CN 109900930A
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- pitch
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Abstract
The present invention discloses a kind of asphalt modification effect evaluation method based on atomic force microscope, comprising the following steps: one, acquisition modified pitch sample；Two, modified pitch sample is placed nitrogen gas concn is to stand 6-10h in 90% guard box and be cooled to room temperature to pitch and be in smooth surface；Three, select silicon probe using 50 μ m, 50 μm of regions in tapping-mode scanning modified pitch sample；Four, atomic force microscope surveys modified pitch two-dimensional surface pattern and 3 d surface topography feature forms image file；Five, PicoView software obtains characterization pitch micro-nano surface roughness features to image file processing；Six, asphalt modification effect assessment is carried out using pitch micro-nano surface roughness features relative change rate and macro-scale modified pitch storage stability and pavement performance relationship.Asphalt modification effect evaluation method of the present invention is easy to operate, convenient and easy, with the cooling bitumen samples of nitrogen protection, avoids asphalt surface by extraneous dust, impurity interference and pollution, guarantees that atomic force tests quality.
Description
Technical field
The invention belongs to pitch micro-properties to evaluate field, change more particularly to a kind of pitch based on atomic force microscope
Property effect evaluation method.
Background technique
(1) with the lasting increase of current amount of traffic, modified pitch using more and more, but how to evaluate changing for pitch
Property effect is the difficult point and emphasis of current research；Due to the limitation of research method and Research scale, asphalt modification effect at present
Evaluation method is mostly macroscopic view test, can not verify the extent of reaction occurred inside modifying agent and pitch；And from the microcosmic spy of pitch
Journal of Sex Research modified pitch can inherently explain the superiority and inferiority of asphalt modification effect and the relationship of its macro property quality, therefore should
The research of method is very necessary.
(2) more and more instruments make it possible that the microcosmic observation of material and analysis, the microscopic characteristics of current pitch are surveyed
Test instrument mainly has fluorescence microscope, scanning electron microscope, atomic force microscope；Wherein the observing result of atomic force microscope is micro-nano
Meter level can obtain the high-precision two-dimensional and 3 d surface topography feature of pitch from nanoscale, analyze modifying agent in pitch
Component is distributed and the mutually material microstructures scene such as separation；Therefore it is complete to can help to researcher for atomic force microscope test method
Recognize to aspect the modification feature of pitch；
Application No. is 201310515741.9 patents to disclose a kind of pitch microscopic characteristics based on atomic force microscope
Research method, including observed for atomic force microscope bitumen samples preparation, surface topography imaging, roughness it is high-precision fixed
Amount analysis and adhesive force analysis: (1) preparation of bitumen samples complies with atomic force microscope observation and requires.(2) surface topography
Imaging method be using atomic force microscope to bitumen samples from two dimension angular with high-resolution from specimen surface selection area
The size and density degree of interior bee shape structure.(3) roughness high-precision quantitative analytic process is to be analyzed using suitable data
Software obtains roughness parameter in atomic force microscope images region.(4) adhesive force analysis is to be obtained using atomic force microscope
Force curve sticks force value by force curve acquisition.It (5) can quantitative assessment pitch adhesion and self-healing using roughness and adhesive force
Performance.It studies asphalt surface pattern by microcosmic angle to analyze the factors such as modification, aging to the microcosmic composed structure of pitch
It influences, and evaluates the adhesion of pitch by surface topography imaging, the analysis of surface roughness high-precision quantitative and adhesion test
And self-healing ability, it needs to carry out complicated operation and sampling and carries out force curve test, be easy to cause biggish error.
Summary of the invention
In response to the problems existing in the prior art, the purpose of the present invention is to provide a kind of pitches based on atomic force microscope to change
Property effect evaluation method.
To achieve the above object, the technical solution adopted by the present invention is that:
A kind of asphalt modification effect evaluation method based on atomic force microscope, comprising the following steps:
(1), modified pitch sample is obtained；
(2), modified pitch sample is placed in the guard box that nitrogen gas concn is 90%, standing 6-10h to pitch is cooled to
Room temperature and be in smooth surface；
(3), selection silicon probe scans the square area of 50 μm of 50 μ m in modified pitch sample using tapping-mode；
(4), the two-dimensional surface pattern and 3 d surface topography feature of modified pitch are obtained using atomic force microscopy mirror device
Image, and formed image file preservation；
(5) the atomic force image file for obtaining matrix pitch is operated according to step (2)-(4)；
(6), image file in step (4) and step (5) is handled using PicoView software, obtains and characterizes the figure
As the roughness features of the pitch micro-nano surface of file area；
(7), the relative change rate using the roughness features of the pitch micro-nano surface and macro-scale modified pitch
Storage stability and the relationship of pavement performance carry out the evaluation of asphalt modification effect.
The variation of microstructure after asphalt modification is analyzed from the surface appearance feature of micro-nano angle research modified pitch,
And the research means of asphalt modification effect are analyzed by two dimension, 3-D image feature and roughness features；Using side of the invention
Method can effectively overcome the shortcomings of present modification pitch macroscopic view test evaluation, mention from the modified effect that microcosmic angle is pitch
For reasonably explaining.
Further, the silicon probe in the step (3) is silicon probe of aluminizing, and needle point radius of curvature < 10nm, the back side is aluminized
Reflecting layer.
Further, roughness features include r.m.s. roughness Rq, average roughness Ra and are averaged in the step (6)
Roughness height Rz.
Further, the evaluation index of the relative change rate in the step (7) are as follows:
Wherein: Δ Rq, Δ Ra, Δ Rz are respectively to be based on r.m.s. roughness Rq, average roughness Ra and average roughness height
Spend the asphalt modification Indexes of Evaluation Effect of Rz；Rq0、Ra0And Rz0The respectively r.m.s. roughness on matrix pitch surface, average thick
Rugosity and average roughness height value；Rq1、Ra1、Rz1The respectively r.m.s. roughness on SBS modified pitch surface, mean roughness
With average roughness height value.
Further, the relative change rate of the roughness features in the step (7) and macro-scale modified pitch store
Stability and the relationship of pavement performance such as table:
Further, the specific steps of the step (1) are as follows:
Matrix pitch is heated to 160 DEG C in molten condition, under the shear rate of 4000r/min, by matrix pitch matter
The SBS modifier of the 3%-8% of amount is added in matrix pitch and shears 60min；
By glass slide after 120 DEG C of baking ovens uniformly preheat 1h, guarantee dry tack free, take 15g molten condition pitch titration in
It is spread out on 22mm × 22mm × 0.8mm glass slide, and it is made uniformly to spread out the circle in 1.5cm.
Compared with prior art, the beneficial effects of the present invention are:
The present invention is a kind of evaluation method of set of asphalt modification effect based on atomic force microscope, combines multinomial arrange
Method is granted, can guarantee that the modified pitch sample surface obtained is smooth clean, is avoided as far as possible extraneous in sample preparation procedure
The interference and pollution of dust, impurity to asphalt surface；Compared to other methods, this method is by obtaining the micro-nano table of modified pitch
The two and three dimensions characteristics of image in face, corresponding roughness variable quantity after calculating it before modified, based on roughness features and macroscopic view
The relationship of scale modified pitch storage stability and pavement performance, can rapidly and efficiently evaluation asphalt modification effect, and have
It is easy to have the advantages that operation and sample prepare.
Detailed description of the invention
Fig. 1 is method flow schematic diagram of the invention；
Fig. 2 is the atomic force microscope observation chart (two dimension) of 70# matrix pitch；
Fig. 3 is the atomic force microscope observation chart (three-dimensional) of 70# matrix pitch；
The atomic force microscope observation chart (two dimension) of Fig. 4 is SBS volume when being 3% modified pitch；
The atomic force microscope observation chart (three-dimensional) of Fig. 5 is SBS volume when being 3% modified pitch；
The atomic force microscope observation chart (two dimension) of Fig. 6 is SBS volume when being 8% modified pitch；
The atomic force microscope observation chart (three-dimensional) of Fig. 7 is SBS volume when being 8% modified pitch；
Specific embodiment
Below in conjunction with the attached drawing in the present invention, technical solution of the present invention is clearly and completely described, it is clear that
Described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the implementation in the present invention
Example, those of ordinary skill in the art's all other embodiment obtained under the conditions of not making creative work belong to
The scope of protection of the invention.
Embodiment 1:
1, sample prepares:
(1) 100g matrix pitch is placed in baking oven and is heated to 160 DEG C in melt-flow state, utilize high speed shear instrument point
The SBS modifier of 3% and 8% (asphalt quality) is not added in matrix pitch, medium shear rate 4000r/min, shearing
Time is 60min；The technology of matrix pitch and SBS are as shown in Table 1 and Table 2.
1 matrix pitch technological property of table
The technological property of 2 SBS of table
(2) glass slide is placed in 120 DEG C of baking ovens and is evenly heated 1h；
(3) the SBS modified pitch in molten state of 15g or so is dripped in 22mm × 22mm × 0.8mm glass slide, and makes it
Uniformly spread out the circle in 1.5cm；
(4) slide specimen prevention nitrogen gas protection box (nitrogen gas concn 90%) natural cooling 6-10h is put into as pitch to try
Sample.
2, atomic force tests asphalt surface pattern
(1) selection is suitably aluminized silicon probe, needle point radius of curvature < 10nm, and the back side is aluminized reflecting layer, to asphalt sample school
It is quasi-；
(2) using the square area of 50 μm of 50 μ m in tapping-mode scanning modified pitch sample；The bullet of cantilever beam
Property constant be 0.4N/m, jib-length 225um, boom width 38um, tip height 12um, sweep speed is
10.09um/s, image analysis rate are 512 × 512；
(3) two dimensional image and 3-D image of modified pitch are obtained using atomic force microscope, and the image of formation is literary
Part saves；
(4) it is handled using the pico view software of Agilent (aglient) company image is obtained, is characterized
R.m.s. roughness Rq, average roughness Ra and the average roughness height Rz of the image-region.
(5) the r.m.s. roughness Rq of the modified front and rear surfaces of pitch SBS, average roughness Ra and average roughness height Rz phase
The evaluation index number of change rate is calculated and includes:
Wherein: Δ Rq, Δ Ra, Δ Rz are respectively based on r.m.s. roughness, mean roughness and average roughness height
Asphalt modification Indexes of Evaluation Effect；Rq0、Ra0And Rz0Respectively the r.m.s. roughness on matrix pitch surface, mean roughness and
Average roughness height value；Rq1、Ra1、Rz1The respectively r.m.s. roughness on SBS modified pitch surface, mean roughness and average
Roughness height value.
The relative change rate of roughness features and macro-scale modified pitch storage stability and the relationship of pavement performance are such as
Table:
Note: according to related data and calculation formula, three indexs are from should numerically approach.When having two in three index values
A or above numerical value can determine that the modified effect of the modified pitch is under the jurisdiction of the variation range all in a variation range
Effect.
(6) according to the roughness features of calculating as a result, with macro-scale modified pitch storage stability and pavement performance
Relationship, the evaluation result for carrying out asphalt modification effect are as shown in table 3.
The test of 3 SBS modified pitch modified effect of table
Note: softening point difference test method is referring to highway engineering pitch and Asphalt Mixture Experiment regulation (JTG E20-
2011)-T0661；Ductility test method is referring to (JTG E20-2011)-T0605；Movement viscosity test method is referring to (JTG
E20-2011)-T0619. relevant regulations are referring to JTG_F40-2017 " standard specification for construction and acceptance of highway asphalt pavement ".
(7) as seen from the above table, 3% SBS is good to the modified effect of pitch, and 8% SBS is to the modified effect of pitch
It is poor.Δ Rq, Δ Ra, Δ Rz value and modified pitch macro property index have preferable relationship, after 40%, value is got over
Greatly, the modified effect of pitch is poorer.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (6)
1. a kind of asphalt modification effect evaluation method based on atomic force microscope, which comprises the following steps:
(1), modified pitch sample is obtained；
(2), modified pitch sample is placed in the guard box that nitrogen gas concn is 90%, standing 6-10h to pitch is cooled to room temperature
It and is in smooth surface；
(3), selection silicon probe scans the square area of 50 μm of 50 μ m in modified pitch sample using tapping-mode；
(4), the two-dimensional surface pattern of modified pitch and the figure of 3 d surface topography feature are obtained using atomic force microscopy mirror device
Picture, and form image file preservation；
(5), the atomic force image file for obtaining matrix pitch is operated according to step (2)-(4)；
(6), the image file in the step (4), step (5) is handled using PicoView software, obtaining characterization should
The roughness features of the pitch micro-nano surface in image file region；
(7), it is stored using the relative change rate of the pitch micro-nano surface roughness features and macro-scale modified pitch steady
Qualitative and pavement performance relationship carries out the evaluation of asphalt modification effect.
2. a kind of asphalt modification effect evaluation method based on atomic force microscope according to claim 1, feature exist
It is silicon probe of aluminizing in, silicon probe in the step (3), needle point radius of curvature < 10nm, the back side is aluminized reflecting layer.
3. a kind of asphalt modification effect evaluation method based on atomic force microscope according to claim 1, feature exist
In roughness features include r.m.s. roughness Rq, average roughness Ra and average roughness height Rz in the step (6).
4. a kind of asphalt modification effect evaluation method based on atomic force microscope according to claim 1, feature exist
In the evaluation index of the relative change rate in the step (7) are as follows:
Wherein: Δ Rq, Δ Ra are respectively the pitch based on r.m.s. roughness Rq, average roughness Ra and average roughness height Rz
Evaluation of modification effect index；Rq0、Ra0And Rz0The respectively r.m.s. roughness on matrix pitch surface, mean roughness and average
Roughness height value；Rq1、Ra1、Rz1The respectively r.m.s. roughness on SBS modified pitch surface, mean roughness and average roughness
Height value.
5. a kind of asphalt modification effect evaluation method based on atomic force microscope according to claim 1, feature exist
In the relative change rate of, step (7) roughness features and macro-scale modified pitch storage stability and pavement performance
Relationship are as follows: relative change rate modified pitch storage stability and pavement performance between 0-50% are excellent, relative change rate in 50-
Modified pitch storage stability and pavement performance are good between 100%, and relative change rate stores in 100% or more modified pitch
Stability and pavement performance are poor.
6. a kind of asphalt modification effect evaluation method based on atomic force microscope according to claim 1, feature exist
In the specific steps of the step (1) are as follows:
Matrix pitch is heated to 160 DEG C in molten condition, under the shear rate of 4000r/min, by matrix pitch quality
The SBS modifier of 3%-8% is added in matrix pitch and shears 60min；
By glass slide after 120 DEG C of baking ovens uniformly preheat 1h, guarantee dry tack free, takes the titration of 15g molten condition pitch in 22mm
It is spread out on × 22mm × 0.8mm glass slide, and it is made uniformly to spread out the circle in 1.5cm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112162116A (en) * | 2020-10-10 | 2021-01-01 | 南京林业大学 | Characterization method for compatibility mechanism of epoxy emulsified asphalt and old asphalt on cold recycled aggregate |
| CN114594240A (en) * | 2022-03-17 | 2022-06-07 | 贵州理工学院 | Method for detecting mixing amount of SBS (styrene butadiene styrene) modifier in modified asphalt based on surface morphology parameters |
| CN115181429A (en) * | 2022-06-16 | 2022-10-14 | 山西省交通科技研发有限公司 | Biological oil modified rubber asphalt and phase separation evaluation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1821743A (en) * | 2006-03-27 | 2006-08-23 | 北京航空航天大学 | Atomic force microscopic detecting method and device for moonscape environment locating measurement |
| CN103529244A (en) * | 2013-10-28 | 2014-01-22 | 东南大学 | Method based on atomic force microscope for researching microscopic characteristics of asphalt |
| CN106199078A (en) * | 2016-06-27 | 2016-12-07 | 上海交通大学 | A kind of active somatic cell surface topography atomic force microscope quick accurate Characterization method |
| 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 |
-
2019
- 2019-03-04 CN CN201910160755.0A patent/CN109900930A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1821743A (en) * | 2006-03-27 | 2006-08-23 | 北京航空航天大学 | Atomic force microscopic detecting method and device for moonscape environment locating measurement |
| CN103529244A (en) * | 2013-10-28 | 2014-01-22 | 东南大学 | Method based on atomic force microscope for researching microscopic characteristics of asphalt |
| CN106199078A (en) * | 2016-06-27 | 2016-12-07 | 上海交通大学 | A kind of active somatic cell surface topography atomic force microscope quick accurate Characterization method |
| 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 |
Non-Patent Citations (4)
| Title |
|---|
| 孙国强等: "基于AFM的沥青微观结构研究进展", 《石油沥青》 * |
| 易军艳等: "基于原子力显微镜技术的沥青与矿料表面粗糙度及黏附特性", 《复合材料学报》 * |
| 杨军等: "沥青原子力显微镜微观图像的特征分析", 《石油学报（石油加工）》 * |
| 马翔等: "２种改性剂对沥青表面形貌的影响", 《建筑材料学报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112162116A (en) * | 2020-10-10 | 2021-01-01 | 南京林业大学 | Characterization method for compatibility mechanism of epoxy emulsified asphalt and old asphalt on cold recycled aggregate |
| CN112162116B (en) * | 2020-10-10 | 2023-08-29 | 南京林业大学 | Characterization method of blending mechanism of epoxy emulsified asphalt and old asphalt on cold regenerated aggregate |
| CN114594240A (en) * | 2022-03-17 | 2022-06-07 | 贵州理工学院 | Method for detecting mixing amount of SBS (styrene butadiene styrene) modifier in modified asphalt based on surface morphology parameters |
| CN115181429A (en) * | 2022-06-16 | 2022-10-14 | 山西省交通科技研发有限公司 | Biological oil modified rubber asphalt and phase separation evaluation method thereof |
| CN115181429B (en) * | 2022-06-16 | 2023-11-14 | 山西省交通科技研发有限公司 | Biological oil modified rubber asphalt and phase separation evaluation method thereof |
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Application publication date: 20190618 |