CN106248998A - 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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- CN106248998A CN106248998A CN201610581285.1A CN201610581285A CN106248998A CN 106248998 A CN106248998 A CN 106248998A CN 201610581285 A CN201610581285 A CN 201610581285A CN 106248998 A CN106248998 A CN 106248998A
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- asphalt
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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)
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- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
Abstract
The present invention relates to a kind of asphalt Research on Mechanical Properties method based on atomic force microscopy, the method comprises the steps: that (1) uses freezing low temperature cutting method to prepare asphalt sample；(2) asphalt sample is observed by the AFM QNM nanoscale mechanical property quantization modules utilizing atomic force microscope, obtaining its mechanical characteristic image, mechanical characteristic image includes modulus properties image, adhesion characteristic image, Dissipated energy characteristic image and deflection characteristic image；(3) use Nanoscope Analysis software respectively each mechanical characteristic image to be carried out quantitative analysis, obtain the modulus value of component to be studied, adhesion values, Dissipated energy value and deformation value.The method that the present invention provides is easy to operation, and can be implemented in and do not separate under each component premise of compound, directly records the mechanical characteristic of the micro-nano-scale of a certain 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 method, especially relate to a kind of based on atomic force microscopy
The asphalt Research on Mechanical Properties method of technology.
Background technology
Along with the popularization and application of Applied of Asphalt Pavement Recycle Technique, the most effectively estimate the surplus value of road-surface milling material, especially
It is the judgement for bituminous cements degree of aging, has become as road researcher issues that need special attention.
Bituminous paving is mainly asphalt, asphalt by Colophonium, gather materials and Particles dispersed that hole forms
Material, its performance is affected, therefore to Colophonium by factors such as each component ratio, traffic micro-simulation and component interphase interactions
The Research on Mechanical Properties of compound is the most more complicated.Current specifications recommends to use the test method of extracting and reclaiming, and not only operation is multiple
Miscellaneous, and result of study can not truly reflect the degree of aging of Colophonium.
Summary of the invention
Defect that the purpose of the present invention is contemplated to overcome above-mentioned prior art to exist and provide a kind of and show based on atomic force
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, the method includes walking as follows
Rapid:
(1) freezing low temperature cutting method is used to prepare asphalt sample；
(2) utilize the AFM-QNM nanoscale mechanical property quantization modules of atomic force microscope to asphalt sample
Be observed, obtain asphalt sample mechanical characteristic image, described mechanical characteristic image include modulus properties image,
Adhesion characteristic image, Dissipated energy characteristic image and deflection characteristic image；
(3) using Nanoscope Analysis software respectively each mechanical characteristic image to be carried out quantitative analysis, acquisition is treated
The research modulus value of component, adhesion values, Dissipated energy value and deformation value.
Step (1) prepare asphalt sample particularly as follows:
(101) test specimen is freezing: wrapped by bitumen mixture specimen preservative film to be studied, cold in cryostat case
Freeze the setting time；
(102) test specimen cutting: under the effect of cooling water, with makita 4100NH, bitumen mixture specimen is cut into Colophonium
Compound sample；
(103) sample cleans: the cuboid asphalt sample of well cutting uses the mineral water of design temperature clean,
Remove surface contaminants；
(104) Storage of sample: be evaporated asphalt specimen surface moisture and asphalt Storage of sample is being contained sample
In Dai.
In step (101), cryostat case temperature is-9 DEG C～-11 DEG C.
In step (101), the setting time was specially more than or equal to 24 hours.
In step (102), test specimen cutting completed in 10 minutes.
In step (103), the temperature of the mineral water of design temperature is 4 DEG C～6 DEG C.
Colophonium is mixed by the AFM-QNM nanoscale mechanical property quantization modules using atomic force microscope in step (2)
When material samples is observed, first choosing one piece of observation area in asphalt sample, that observes in this observation area is every
The force curve shape of individual pixel, and then obtain the mechanical characteristic image of whole observation area.
Step (2) uses the AFM-QNM nanoscale mechanical property quantization modules of atomic force microscope to asphalt
Sample is observed carrying out under 25 DEG C of temperature conditionss.
The method is used when a certain asphalt sample is carried out Research on Mechanical Properties, to obtain the mixing of at least one Colophonium
Material samples sample, and each Colophonium bulk testing sample is chosen multiple observation area, obtain respectively in each sample and respectively observe
The modulus value in region, adhesion values, Dissipated energy value and deformation value, finally ask for the average mould as this asphalt sample
Value, adhesion values, Dissipated energy value and deformation value.
Compared with prior art, present invention have the advantage that
(1) present invention uses atomic force microscopy to realize not separating on the premise of asphalt respectively forms, directly
Record the mechanical characteristic of one-component, provide from the mechanical characteristic of micro-nano-scale quantization signifying asphalt for researcher
A kind of new method；
(2) cryostat case temperature of the present invention is-9 DEG C～-11 DEG C, and the time that sets is specially more than or equal to 24 hours,
Suitably temperature and cooling time ensure that asphalt sample mass is good, it is ensured that follow-up employing atomic force microscope is entered
Row observation also obtains mechanical characteristic image well, can improve the accuracy of follow-up mechanical characteristic numerical value；
(3) asphalt sample preparation of the present invention is simple, it is simple to operation, and wherein test specimen cutting is complete in 10 minutes
Become to be prevented from because cutting produces heat effect, cause the softening of asphalt sample, affect flatness and the light of specimen surface
Cleanliness, and then affect the accuracy of follow-up mechanical characteristic numerical value；
(4) present invention uses the AFM-QNM nanoscale mechanical property quantization modules of atomic force microscope to mix Colophonium
Obtain each pixel to observation area when material samples is observed and be observed its force curve image, thus ensure to obtain
Mechanical characteristic image more efficient；
(5) carry out under 25 DEG C of temperature conditionss when the present invention uses atomic force microscope to be observed, it is ensured that suitably temperature
It is relatively reliable effectively that degree enables to observed result；
(6) certain asphalt sample is carried out using multisample during Research on Mechanical Properties by the present invention, and many observation areas are entered
Row repetitive measurement takes the method for average, it is to avoid randomness, improves the accuracy of end product.
Accompanying drawing explanation
Fig. 1 is the FB(flow block) of asphalt Research on Mechanical Properties method of the present invention；
Fig. 2 be Peak force QNM of the present invention tap circulation middle probe and sample effect process schematic process and
Power-curve；
Fig. 3 is the mechanical characteristic image in " territory, black glue region " in asphalt sample of the present invention；
Fig. 4 is concrete modulus scattergram in modulus properties image of the present invention；
Fig. 5 is the average modulus curve scattergram in asphalt component of the present invention each pixel region.
Detailed description of the invention
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment
As it is shown in figure 1, a kind of asphalt Research on Mechanical Properties method based on atomic force microscopy, the method bag
Include following steps:
Step 1: use freezing low temperature cutting method to prepare asphalt sample, specifically includes following steps:
(101) test specimen is freezing: wrapped by bitumen mixture specimen preservative film to be studied, cold in cryostat case
Freezing the setting time, cryostat case temperature is-9 DEG C～-11 DEG C, and in the present embodiment, the warmest household freezer temperature is-10 DEG C, time freezing
Between more than or equal to 24 hours.
(102) test specimen cutting: under the effect of cooling water, with makita 4100NH bitumen mixture specimen is cut into 30 ×
20 × 10mm cuboid asphalt sample, test specimen cutting completed in 10 minutes, prevented from, because cutting produces heat effect, causing
The softening of Colophonium composite sample, affects flatness and the fineness of specimen surface, and then affects the standard of follow-up mechanical characteristic numerical value
Really property.
(103) sample cleans: the cuboid asphalt sample of well cutting uses the mineral water of design temperature clean,
Removing surface contaminants, wherein the temperature of mineral water is 4 DEG C～6 DEG C, and this enforcement mineral water temperature is 5 DEG C.
(104) Storage of sample: be evaporated asphalt specimen surface moisture and asphalt Storage of sample is being contained sample
In Dai.
Step 2: utilize the QNM nanoscale mechanical property based on peak force tapping-mode of atomic force microscope (AFM)
Asphalt sample is observed by quantization modules (AFM-QNM nanoscale mechanical property quantization modules), obtains Colophonium and mixes
Closing the mechanical characteristic image of material samples, described mechanical characteristic image includes modulus properties image, adhesion characteristic image, dissipation
Energy characteristic image and deflection characteristic image, specifically, first choose one piece of observation area in asphalt sample, observation
The force curve shape of each pixel in this observation area, and then obtain the mechanical characteristic image of whole observation area, whole
The acquisition of observation and mechanical characteristic image is carried out under 25 DEG C of temperature conditionss.
Step 3: use Nanoscope Analysis software respectively each mechanical characteristic image to be carried out quantitative analysis, obtain
The modulus value of component to be studied, adhesion values, Dissipated energy value and deformation value, Nanoscope Analysis software is atomic force
The analysis software that microscope carries.
The method is used when a certain asphalt sample is carried out Research on Mechanical Properties, to obtain the mixing of at least one Colophonium
Material samples sample, and each Colophonium bulk testing sample is chosen multiple observation area, obtain respectively in each sample and respectively observe
The modulus value in region, adhesion values, Dissipated energy value and deformation value, finally ask for the average mould as this asphalt sample
Value, adhesion values, Dissipated energy value and deformation value.
The present embodiment Atom force microscope is the ICON model of Brooker company of Germany, selects Peak Force QNM work
Operation mode." territory, black glue region " in observation area selection asphalt sample, i.e. asphalt mastic component carry out mechanical characteristic and divide
Analysis, utilizes the Peak force QNM module of atomic force microscope, and in this scan pattern, probe passes through piezoelectric ceramics
Part, a driven atom force microscope cantilever makes probe move, and probe often contacts a sample, i.e. produces a force curve, and test is adopted
With silicon nitride cantilevers probe, sample is scanned imaging, sweep limits 5 × 5um2, image slices vegetarian refreshments 512 × 512, test temperature
Spend 25 DEG C.Finally, the mechanical characteristic surveying observation area is presented in the form of images.
In mono-tapping of Peak force QNM circulation middle probe and sample effect process schematic such as Fig. 2 (a) institute
Showing, 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, (3)-(4)-(5) represent after probe and sample interact, leave the process of sample；By real-time power-
The Fitting Analysis of curve, can obtain the corresponding mechanical information of sample.In Peak force QNM circulates, owing to peak force is non-
The least, contact similar hard sphere and elastic linear between probe with sample, it may be considered that utilize in contact mechanics DMT model to power
Curve is fitted analyzing, and obtains the Young's modulus of sample；Utilize the graviational interaction between needle point and sample atoms, can be at Massa Medicata Fermentata
Obtaining reflecting the adhesion of sample adhesion characteristics on line, the healing ability of the biggest representative sample of adhesion is the best；Due to peak force
The effect of load makes sample be deformed, the maximum deformation quantity of probe press-in sample, can directly read in power-curve；To Fig. 2
B area that () middle probe approaches and withdraws between two power-curves of sample is integrated, in available tapping circulation
The energy dissipated, i.e. Dissipated energy.Asphalt is gathered materials the multicomponent composite materials formed by Colophonium, breeze, thickness, due to
Mutual embedded squeezing between each component, boundary the clearest and the most definite between the most each component, utilize macro-test method at compound
It is impossible that middle test obtains the character of one-component, and utilize atomic force microscopy realize this idea be one non-
The most readily thing.Fig. 3 is in the asphalt sample utilizing Peak Force QNM module testing to obtain " territory, black glue region "
Mechanical characteristic image, wherein Fig. 3 (a) is modulus properties image, and 3 (b) is adhesion characteristic image, and Fig. 3 (c) is that deflection is special
Property image, Fig. 3 (d) is Dissipated energy characteristic image.Owing to the mechanical characteristics such as Colophonium and the modulus of breeze two component, adhesion exist
Significantly difference, this species diversity can be presented by atomic force microscopy in the form of images, as it is shown on figure 3, colour-difference
The different difference representing mechanical characteristic.The region that in image, modulus is low, adhesion is big is close to asphalt component, and modulus is big and adhesion is little
Region be close to the difference that the difference of breeze or fine aggregate component mechanical characteristic implys that between component.
Statistical analysis software Nanoscope Analysis software subsidiary for AFM can be to the mechanics of the regional area of image
Characteristic carries out quantitative analysis, thus obtains obtaining the modulus value of composition to be studied, adhesion values, Dissipated energy value and deformation value.
As a example by Fig. 3 (a) modulus properties image, choose the region prolonging the direction of arrow in image, as shown in Figure 4, extract corresponding pixel points
Modulus value, obtain the modulus distributed image in the direction of arrow, as shown in Figure 4.As shown in Figure 4, the regional area chosen, the left side
Being to gather materials or breeze contour modulus component region, the right is asphalt component low modulus region, and modulus curve is along with component
There is significant difference in difference.In high-modulus region, the distribution 1.0～4.4GPa of modulus, and divide in low modulus region modulus
Cloth scope is 402～510MPa；In asphalt component and fine aggregate or breeze component interface, there is sudden change in modulus curve.
In order to quantization signifying asphalt component is at the modulus value of the micro-nano-scale of test, select at random in modulus properties image
Take the pixel region of 6 formed objects, utilize Nanoscope Analysis software to obtain the average in each pixel region
Modulus, drafting pattern 5.As shown in Figure 5, the average in different pixels point region fluctuates between 420～510MPa, takes 6 the most again
Average 450MPa in individual different pixels point region, as the modulus value of asphalt component.The present embodiment uses a Colophonium mixing
Material samples sample is observed, naturally it is also possible to use multiple, so that result is relatively reliable.
Claims (9)
1. an asphalt Research on Mechanical Properties method based on atomic force microscopy, it is characterised in that the method bag
Include following steps:
(1) freezing low temperature cutting method is used to prepare asphalt sample；
(2) asphalt sample is carried out by the AFM-QNM nanoscale mechanical property quantization modules utilizing atomic force microscope
Observation, obtains the mechanical characteristic image of asphalt sample, and described mechanical characteristic image includes modulus properties image, adhesion
Force characteristic image, Dissipated energy characteristic image and deflection characteristic image；
(3) use Nanoscope Analysis software respectively each mechanical characteristic image to be carried out quantitative analysis, obtain to be studied
The modulus value of component, adhesion values, Dissipated energy value and deformation value.
A kind of asphalt Research on Mechanical Properties method based on atomic force microscopy the most according to claim 1,
It is characterized in that, step (1) prepare asphalt sample particularly as follows:
(101) test specimen is freezing: being wrapped by bitumen mixture specimen preservative film to be studied, in cryostat case, freezing sets
Fix time；
(102) test specimen cutting: under the effect of cooling water, cuts into Colophonium with makita 4100NH by bitumen mixture specimen and mixes
Material samples；
(103) sample cleans: the cuboid asphalt sample of well cutting uses the mineral water of design temperature clean, removes
Surface contaminants；
(104) Storage of sample: be evaporated asphalt specimen surface moisture and by asphalt Storage of sample in containing sample bag.
A kind of asphalt Research on Mechanical Properties method based on atomic force microscopy the most according to claim 2,
It is characterized in that, in step (101), cryostat case temperature is-9 DEG C～-11 DEG C.
A kind of asphalt Research on Mechanical Properties method based on atomic force microscopy the most according to claim 2,
It is characterized in that, in step (101), the setting time was specially more than or equal to 24 hours.
A kind of asphalt Research on Mechanical Properties method based on atomic force microscopy the most according to claim 2,
It is characterized in that, in step (102), test specimen cutting completed in 10 minutes.
A kind of asphalt Research on Mechanical Properties method based on atomic force microscopy the most according to claim 2,
It is characterized in that, in step (103), the temperature of the mineral water of design temperature is 4 DEG C～6 DEG C.
A kind of asphalt Research on Mechanical Properties method based on atomic force microscopy the most according to claim 1,
It is characterized in that, step (2) uses the AFM-QNM nanoscale mechanical property quantization modules of atomic force microscope Colophonium is mixed
When conjunction material samples is observed, first chooses one piece of observation area in asphalt sample, observe in this observation area
The force curve shape of each pixel, and then obtain the mechanical characteristic image of whole observation area.
A kind of asphalt Research on Mechanical Properties method based on atomic force microscopy the most according to claim 1,
It is characterized in that, step (2) uses the AFM-QNM nanoscale mechanical property quantization modules of atomic force microscope to mix Colophonium
Material samples is observed carrying out under 25 DEG C of temperature conditionss.
A kind of asphalt Research on Mechanical Properties method based on atomic force microscopy the most according to claim 1,
It is characterized in that, use the method when a certain asphalt sample is carried out Research on Mechanical Properties, to obtain at least one Colophonium and mix
Close material samples sample, and each Colophonium bulk testing sample is chosen multiple observation area, obtain respectively in each sample and respectively see
Survey the modulus value in region, adhesion values, Dissipated energy value and deformation value, finally ask for average as this asphalt sample
Modulus value, adhesion values, Dissipated energy value and deformation value.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107064475A (en) * | 2017-05-03 | 2017-08-18 | 同济大学 | Ageing of asphalt degree based on atomic force microscopy method of discrimination in situ |
| CN109932529A (en) * | 2019-03-08 | 2019-06-25 | 河海大学 | A method of based on polymer dispersity in atomic force microscope detection SBS modified pitch |
| 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 |
| CN110687318A (en) * | 2018-07-06 | 2020-01-14 | 多氟多化工股份有限公司 | Analysis method of copper dendrite on surface of diaphragm |
| 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 |
| 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 |
| 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 |
| CN112755578A (en) * | 2020-12-22 | 2021-05-07 | 同济大学 | Asphalt cement separation method based on supercritical fluid extraction |
| CN113607608A (en) * | 2021-09-02 | 2021-11-05 | 交通运输部公路科学研究所 | Method for evaluating interaction capacity of cement emulsified asphalt mortar and old asphalt interface |
| 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 |
| CN114324983A (en) * | 2022-01-06 | 2022-04-12 | 同济大学 | Method and system for quantifying fusion degree of new asphalt and old asphalt in hot recycled asphalt mixture |
| CN116007983A (en) * | 2022-12-05 | 2023-04-25 | 北京建筑大学 | Method for sampling aged asphalt by layering slices |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107064475A (en) * | 2017-05-03 | 2017-08-18 | 同济大学 | Ageing of asphalt degree based on atomic force microscopy method of discrimination in situ |
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| CN110687318A (en) * | 2018-07-06 | 2020-01-14 | 多氟多化工股份有限公司 | Analysis method of copper dendrite on surface of diaphragm |
| CN109932529A (en) * | 2019-03-08 | 2019-06-25 | 河海大学 | A method of based on polymer dispersity in atomic force microscope detection SBS modified pitch |
| 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 |
| 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 |
| 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 |
| CN112755578A (en) * | 2020-12-22 | 2021-05-07 | 同济大学 | Asphalt cement separation method based on supercritical fluid extraction |
| CN113607608A (en) * | 2021-09-02 | 2021-11-05 | 交通运输部公路科学研究所 | Method for evaluating interaction capacity of cement emulsified asphalt mortar and old asphalt interface |
| 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 |
| CN114324983A (en) * | 2022-01-06 | 2022-04-12 | 同济大学 | Method and system for quantifying fusion degree of new asphalt and old asphalt in hot recycled asphalt mixture |
| 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 |
| CN116007983A (en) * | 2022-12-05 | 2023-04-25 | 北京建筑大学 | Method for sampling aged asphalt by layering slices |
| 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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