CN106248998B - A kind of asphalt Research on Mechanical Properties method based on atomic force microscopy - Google Patents
A kind of asphalt Research on Mechanical Properties method based on atomic force microscopy Download PDFInfo
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- CN106248998B CN106248998B CN201610581285.1A CN201610581285A CN106248998B CN 106248998 B CN106248998 B CN 106248998B CN 201610581285 A CN201610581285 A CN 201610581285A CN 106248998 B CN106248998 B CN 106248998B
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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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Radiology & Medical Imaging (AREA)
- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
Abstract
The asphalt Research on Mechanical Properties method based on atomic force microscopy that the present invention relates to a kind of, this method comprises the following steps: (1) preparing asphalt sample using freezing low temperature cutting method；(2) asphalt sample is observed using the AFM-QNM nanoscale mechanical property quantization modules of atomic force microscope, its mechanical characteristic image is obtained, mechanical characteristic image includes modulus properties image, adhesion strength characteristic image, Dissipated energy characteristic image and deflection characteristic image；(3) quantitative analysis is carried out to each mechanical characteristic image respectively using Nanoscope Analysis software, obtains modulus value, adhesion values, Dissipated energy value and the deformation value of component to be studied.Method provided by the invention is easy to operation, and may be implemented directly to measure the mechanical characteristic of the micro-nano-scale of a certain component under the premise of not separating mixture each component, differentiates in situ for asphalt performance and lays a good foundation.
Description
Technical field
The present invention relates to a kind of asphalt Research on Mechanical Properties methods, are based on atomic force microscopy more particularly, to one kind
The asphalt Research on Mechanical Properties method of technology.
Background technique
With the popularization and application of Applied of Asphalt Pavement Recycle Technique, the surplus value of road-surface milling material how is effectively estimated, especially
It is the judgement for bituminous cements degree of aging, has become road researcher's issues that need special attention.
Bituminous pavement is mainly asphalt, asphalt by pitch, gather materials the Particles dispersed formed with hole
Material, performance are influenced by the factors such as interaction between each component ratio, traffic micro-simulation and component, therefore to pitch
The Research on Mechanical Properties of mixture is also more complicated.Current specifications is recommended to use the test method of extracting and reclaiming, and not only operation is multiple
It is miscellaneous, and result of study cannot really reflect the degree of aging of pitch.
Summary of the invention
It is aobvious based on atomic force that it is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind
The asphalt Research on Mechanical Properties method of microtechnology.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of asphalt Research on Mechanical Properties method based on atomic force microscopy, this method include following step
It is rapid:
(1) asphalt sample is prepared using freezing low temperature cutting method；
(2) using the AFM-QNM nanoscale mechanical property quantization modules of atomic force microscope to asphalt sample
Be observed, obtain asphalt sample mechanical characteristic image, the mechanical characteristic image include modulus properties image,
Adhesion strength characteristic image, Dissipated energy characteristic image and deflection characteristic image；
(3) using Nanoscope Analysis software respectively to each mechanical characteristic image carry out quantitative analysis, obtain to
Study modulus value, adhesion values, Dissipated energy value and the deformation value of component.
Step (1) prepares asphalt sample specifically:
(101) test specimen freezes: bitumen mixture specimen to be studied is wrapped with preservative film, it is cold in cryostat case
Freeze setting time；
(102) test specimen is cut: under the action of cooling water, bitumen mixture specimen being cut into pitch with makita 4100NH
Mixture sample；
(103) sample cleans: the cuboid asphalt sample of well cutting is cleaned using the mineral water of set temperature,
Remove surface contaminants；
(104) Storage of sample: being evaporated asphalt specimen surface moisture and asphalt Storage of sample is being contained sample
In bag.
Cryostat case temperature is -9 DEG C~-11 DEG C in step (101).
Setting time is specially and is greater than or equal to 24 hours in step (101).
Test specimen cutting is completed in 10 minutes in step (102).
The temperature of the mineral water of set temperature is 4 DEG C~6 DEG C in step (103).
Pitch is mixed using the AFM-QNM nanoscale mechanical property quantization modules of atomic force microscope in step (2)
When material sample is observed, one piece of observation area in asphalt sample is chosen first, is observed every in the observation area
The force curve shape of a pixel, and then obtain the mechanical characteristic image of entire observation area.
Step (2) is using the AFM-QNM nanoscale mechanical property quantization modules of atomic force microscope to asphalt
Sample, which is observed, to be carried out under the conditions of 25 DEG C of temperature.
The mixing of at least one pitch is obtained when carrying out Research on Mechanical Properties to a certain asphalt sample using this method
Expect sample sample, and multiple observation areas are chosen to each pitch bulk testing sample, obtains respectively observed in each sample respectively
Modulus value, adhesion values, Dissipated energy value and the deformation value in region, finally seek mould of the mean value as the asphalt sample
Magnitude, adhesion values, Dissipated energy value and deformation value.
Compared with prior art, the present invention has the advantage that
(1) present invention is realized under the premise of not separating asphalt and respectively forming, directly using atomic force microscopy
The mechanical characteristic of one-component is measured, is provided for researcher from the mechanical characteristic of micro-nano-scale quantization signifying asphalt
A kind of new method；
(2) cryostat case temperature of the present invention is -9 DEG C~-11 DEG C, and setting time is specially to be greater than or equal to 24 hours,
Suitable temperature and cooling time can guarantee that asphalt sample mass is good, guarantee it is subsequent using atomic force microscope into
Row is observed and obtains that mechanical characteristic image is good, and the accuracy of subsequent mechanical characteristic numerical value can be improved；
(3) asphalt sample preparation of the present invention is simple, and convenient for operation, wherein test specimen cutting is complete in 10 minutes
At can prevent because cutting generate fuel factor, lead to the softening of asphalt sample, influence the flatness and light of specimen surface
Cleanliness, and then influence the accuracy of subsequent mechanical characteristic numerical value；
(4) present invention mixes pitch using the AFM-QNM nanoscale mechanical property quantization modules of atomic force microscope
Material sample obtains when being observed and is observed its force curve image to each pixel of observation area, to guarantee to obtain
Mechanical characteristic image it is more efficient；
(5) it is carried out under the conditions of 25 DEG C of temperature when the present invention is observed using atomic force microscope, guarantees suitable temperature
Degree enables to observed result relatively reliable effectively；
(6) present invention to certain asphalt sample carry out Research on Mechanical Properties when use multisample, more observation areas into
Row repeatedly measures the method for taking mean value, avoids randomness, improves the accuracy of final result.
Detailed description of the invention
Fig. 1 is the flow diagram of asphalt Research on Mechanical Properties method of the present invention；
Fig. 2 be mono- percussion circulation middle probe of Peak force QNM of the present invention and sample effect process schematic process and
Power-curve；
Fig. 3 is the mechanical characteristic image in " black glue region " in asphalt sample of the present invention；
Fig. 4 is specific modulus distribution map in modulus properties image of the present invention；
Fig. 5 is the mean value modulus curve distribution map in each pixel region of asphalt component of the present invention.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment
As shown in Figure 1, a kind of asphalt Research on Mechanical Properties method based on atomic force microscopy, this method packet
Include following steps:
Step 1: asphalt sample being prepared using freezing low temperature cutting method, is specifically comprised the following steps:
(101) test specimen freezes: bitumen mixture specimen to be studied is wrapped with preservative film, it is cold in cryostat case
Freeze setting time, cryostat case temperature is -9 DEG C~-11 DEG C, and very warm household freezer temperature is -10 DEG C in the present embodiment, when freezing
Between be greater than or equal to 24 hours.
(102) test specimen is cut: under the action of cooling water, bitumen mixture specimen is cut into 30 with makita 4100NH ×
20 × 10mm cuboid asphalt sample, test specimen cutting are completed in 10 minutes, are prevented from generating fuel factor because of cutting, be caused
The softening of pitch composite sample influences the flatness and finish of specimen surface, and then influences the standard of subsequent mechanical characteristic numerical value
True property.
(103) sample cleans: the cuboid asphalt sample of well cutting is cleaned using the mineral water of set temperature,
Surface contaminants are removed, wherein the temperature of mineral water is 4 DEG C~6 DEG C, this implementation mineral spring coolant-temperature gage is 5 DEG C.
(104) Storage of sample: being evaporated asphalt specimen surface moisture and asphalt Storage of sample is being contained sample
In bag.
Step 2: utilizing the QNM nanoscale mechanical property based on peak force tapping-mode of atomic force microscope (AFM)
Quantization modules (AFM-QNM nanoscale mechanical property quantization modules) are observed asphalt sample, and it is mixed to obtain pitch
The mechanical characteristic image of material sample is closed, the mechanical characteristic image includes modulus properties image, adhesion strength characteristic image, dissipates
Energy characteristic image and deflection characteristic image, specifically, one piece of observation area first in selection asphalt sample, observation
The force curve shape of each pixel in the observation area, and then the mechanical characteristic image of entire observation area is obtained, entirely
Observation and the acquisition of mechanical characteristic image carry out under the conditions of 25 DEG C of temperature.
Step 3: quantitative analysis being carried out to each mechanical characteristic image respectively using Nanoscope Analysis software, is obtained
Modulus value, adhesion values, Dissipated energy value and the deformation value of component to be studied, Nanoscope Analysis software are atomic force
The included analysis software of microscope.
The mixing of at least one pitch is obtained when carrying out Research on Mechanical Properties to a certain asphalt sample using this method
Expect sample sample, and multiple observation areas are chosen to each pitch bulk testing sample, obtains respectively observed in each sample respectively
Modulus value, adhesion values, Dissipated energy value and the deformation value in region, finally seek mould of the mean value as the asphalt sample
Magnitude, adhesion values, Dissipated energy value and deformation value.
Atomic force microscope is the ICON model of German Brooker company in the present embodiment, selects Peak Force QNM work
Operation mode.Observation area selects " the black glue region " in asphalt sample, i.e. asphalt mastic component carries out mechanical characteristic point
Analysis, using the Peak force QNM module of atomic force microscope, in this scan pattern, probe passes through piezoelectric ceramics
Part, a driven atom force microscope cantilever keep probe mobile, and a probe sample of every contact generates a force curve, test is adopted
Imaging, 5 × 5um of scanning range are scanned to sample with silicon nitride cantilevers probe2, image slices vegetarian refreshments 512 × 512, test temperature
25 DEG C of degree.Finally, the mechanical characteristic for surveying observation area is showed in the form of images.
In mono- tapping circulation middle probe of Peak force QNM and sample effect process schematic such as Fig. 2 (a) institute
Show, Fig. 2 (b) is the real-time force-curve collected in a tapping circulation.Wherein (1)-(2)-(3) represent probe and approach
The process of sample leaves the process of sample after (3)-(4)-(5) represent probe and sample interacts；By real-time power-
The Fitting Analysis of curve, the available corresponding mechanical information of sample.In Peak force QNM circulation, since peak force is non-
It is often small, similar hard sphere and elastic linear are contacted between probe and sample, it may be considered that using DMT model in contact mechanics to power song
Line is fitted analysis, obtains the Young's modulus of sample；It, can be in force curve using the graviational interaction between needle point and sample atoms
On obtain the adhesion strength of reflection sample adhesion characteristics, the healing ability of the bigger representative sample of adhesion strength is better；Due to peak force lotus
The effect of load is deformed sample, and probe is pressed into the maximum deformation quantity of sample, can directly read in power-curve；To Fig. 2
(b) area that middle probe approaches and withdraw between two power-curves of sample is integrated, and can be obtained in a tapping circulation
The energy of dissipation, i.e. Dissipated energy.Asphalt is gathered materials the multicomponent composite materials formed by pitch, miberal powder, thickness, due to
Mutual embedded squeezing between each component, macroscopically there is no specific boundaries between each component, using macro-test method in mixture
It is impossible that middle test, which obtains the property of one-component, and realizes that this idea is one non-using atomic force microscopy
Normal easy thing.Fig. 3 is in the asphalt sample obtained using Peak Force QNM module testing " black glue region "
Mechanical characteristic image, wherein Fig. 3 (a) is modulus properties image, and 3 (b) be adhesion strength characteristic image, and Fig. 3 (c) is that deflection is special
Property image, Fig. 3 (d) be Dissipated energy characteristic image.Since the mechanical characteristics such as pitch and modulus, the adhesion strength of two component of miberal powder exist
Significant difference, atomic force microscopy can show this species diversity in the form of images, as shown in figure 3, colour-difference
The different difference for representing mechanical characteristic.The intimate asphalt component in the region that modulus is low in image, adhesion strength is big, modulus is big and adhesion strength is small
The intimate miberal powder in region or the difference of fine aggregate component mechanical characteristic imply that the difference between component.
AFM subsidiary statistical analysis software Nanoscope Analysis software can be to the mechanics of the regional area of image
Characteristic carries out quantitative analysis, to obtain obtaining modulus value, adhesion values, Dissipated energy value and the deformation value of composition to be studied.
By taking Fig. 3 (a) modulus properties image as an example, the region for prolonging arrow direction in image is chosen, as shown in figure 4, extracting corresponding pixel points
Modulus value, obtain modulus in the distributed image of arrow direction, as shown in Figure 4.As shown in Figure 4, the regional area chosen, the left side
It is gather materials either high modulus component region, the right such as miberal powder is the low modulus region of asphalt component, modulus curve is with component
There is significant difference in difference.In high-modulus region, 1.0~4.4GPa of distribution of modulus, and in low modulus region modulus point
Cloth range is 402~510MPa；It is mutated in asphalt component and fine aggregate or miberal powder component interface, modulus curve.
In order to which quantization signifying asphalt component is in the modulus value of the micro-nano-scale of test, selected at random in modulus properties image
The pixel region for taking 6 same sizes obtains the mean value in each pixel region using Nanoscope Analysis software
Modulus, drafting pattern 5.As shown in Figure 5, the mean value in different pixels point region fluctuates between 420~510MPa, then takes 6 again
The mean value 450MPa in a different pixels point region, the modulus value as asphalt component.Using a pitch mixing in the present embodiment
Material sample sample is observed, naturally it is also possible to which use is multiple, so that result is relatively reliable.
Claims (4)
1. a kind of asphalt Research on Mechanical Properties method based on atomic force microscopy, which is characterized in that this method packet
Include following steps:
(1) asphalt sample is prepared using freezing low temperature cutting method；
(2) asphalt sample is carried out using the AFM-QNM nanoscale mechanical property quantization modules of atomic force microscope
Observation, obtains the mechanical characteristic image of asphalt sample, and the mechanical characteristic image includes modulus properties image, adherency
Force characteristic image, Dissipated energy characteristic image and deflection characteristic image；
(3) quantitative analysis is carried out to each mechanical characteristic image respectively using Nanoscope Analysis software, obtained to be studied
Modulus value, adhesion values, Dissipated energy value and the deformation value of component；
Step (1) prepares asphalt sample specifically:
(101) test specimen freezes: bitumen mixture specimen to be studied being wrapped with preservative film, freezes and sets in cryostat case
It fixes time, cryostat case temperature is -9 DEG C~-11 DEG C, and setting time is specially to be greater than or equal to 24 hours；
(102) test specimen is cut: under the action of cooling water, bitumen mixture specimen being cut into pitch with makita 4100NH and is mixed
Expect sample, test specimen cutting is completed in 10 minutes；
(103) sample cleans: the cuboid asphalt sample of well cutting being cleaned using the mineral water of set temperature, is removed
Surface contaminants, the temperature of mineral water are 4 DEG C~6 DEG C；
(104) Storage of sample: it is evaporated asphalt specimen surface moisture and by asphalt Storage of sample in containing sample bag.
2. a kind of asphalt Research on Mechanical Properties method based on atomic force microscopy according to claim 1,
It is characterized in that, mixed to pitch using the AFM-QNM nanoscale mechanical property quantization modules of atomic force microscope in step (2)
When conjunction material sample is observed, one piece of observation area in asphalt sample is chosen first, is observed in the observation area
The force curve shape of each pixel, and then obtain the mechanical characteristic image of entire observation area.
3. a kind of asphalt Research on Mechanical Properties method based on atomic force microscopy according to claim 1,
It is characterized in that, step (2) mixes pitch using the AFM-QNM nanoscale mechanical property quantization modules of atomic force microscope
Material sample, which is observed, to be carried out under the conditions of 25 DEG C of temperature.
4. a kind of asphalt Research on Mechanical Properties method based on atomic force microscopy according to claim 1,
It is mixed that at least one pitch is obtained when it is characterized in that, carrying out Research on Mechanical Properties to a certain asphalt sample using this method
Material sample sample is closed, and multiple observation areas are chosen to each asphalt sample sample, is obtained in each sample respectively
Modulus value, adhesion values, Dissipated energy value and the deformation value of each observation area are finally sought mean value and are tried as the asphalt
Modulus value, adhesion values, Dissipated energy value and the deformation value of sample.
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| CN107064475B (en) * | 2017-05-03 | 2020-08-14 | 同济大学 | In-situ discrimination method for asphalt aging degree in mixture based on atomic force microscopy |
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| CN109932529B (en) * | 2019-03-08 | 2020-12-25 | 河海大学 | Method for detecting polymer dispersibility in SBS modified asphalt based on atomic force microscope |
| 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 |
| CN110717510A (en) * | 2019-09-03 | 2020-01-21 | 天津大学 | Material distinguishing method based on deep learning and atomic force microscope force curve |
| CN111855565B (en) * | 2020-07-21 | 2022-09-16 | 南京林业大学 | Method for testing effective mixing amount of direct-vat-set high-viscosity asphalt modifier |
| CN112146962A (en) * | 2020-10-21 | 2020-12-29 | 盐城工学院 | Preparation method of test sample for quantitatively characterizing morphological characteristics of inorganic filler particles |
| CN112755578B (en) * | 2020-12-22 | 2022-05-20 | 同济大学 | Asphalt cement separation method based on supercritical fluid extraction |
| CN113607608B (en) * | 2021-09-02 | 2023-05-12 | 交通运输部公路科学研究所 | Method for evaluating interfacial interaction capability of cement emulsified asphalt cement and old asphalt |
| CN113720703A (en) * | 2021-09-15 | 2021-11-30 | 南京林业大学 | Method for researching mechanism of graphene for enhancing mechanical properties of asphalt |
| CN114324983B (en) * | 2022-01-06 | 2023-09-22 | 同济大学 | Quantification method and system for new and old asphalt fusion degree in heat regeneration asphalt mixture |
| CN116007983B (en) * | 2022-12-05 | 2023-08-04 | 北京建筑大学 | Method for sampling aged asphalt by layering slices |
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| JP2012063319A (en) * | 2010-09-17 | 2012-03-29 | Toppan Printing Co Ltd | Atomic force microscope observation method of polymeric material at high temperature state |
| CN103529244A (en) * | 2013-10-28 | 2014-01-22 | 东南大学 | Method based on atomic force microscope for researching microscopic characteristics of asphalt |
| CN103901231A (en) * | 2014-04-08 | 2014-07-02 | 东南大学 | Preparation method for asphalt sample suitable for atomic force microscope observation |
| 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 |
| CN105628979A (en) * | 2016-02-29 | 2016-06-01 | 东南大学 | Method of characterizing aggregate and asphalt adhesion |
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