CN111307572B - Small-angle neutron scattering-based filled rubber structure network evolution determination method - Google Patents
Small-angle neutron scattering-based filled rubber structure network evolution determination method Download PDFInfo
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Abstract
The invention discloses a filling rubber structure network evolution measuring method based on small-angle neutron scattering. The method comprises the following steps: firstly, preparing a vulcanized filled rubber sample, placing the filled rubber sample to be tested on an in-situ stretching small-angle neutron scattering sample table, carrying out static and in-situ stretching small-angle neutron scattering tests on the filled rubber sample to be tested at different distances from the sample to a detector, carrying out background subtraction and intensity correction treatment on obtained experimental data to obtain a static absolute intensity curve, a dynamic relative intensity curve and a stretching mechanical curve corresponding to the static absolute intensity curve and the dynamic relative intensity curve, and finally obtaining structural evolution information of the filled rubber sample to be tested through model fitting calculation. The method for measuring the network evolution of the filled rubber structure has the advantages of in-situ, rapidness, effectiveness, directness and comprehensiveness, and can be used for further and deeply exploring the influence of the micro morphological characteristics of the filled rubber on the mechanical property of the filled rubber.
Description
Technical Field
The invention belongs to the field of nuclear technology application, and particularly relates to a filling rubber structure network evolution measuring method based on small-angle neutron scattering.
Background
The rubber can greatly improve the mechanical properties such as modulus, tensile strength, breaking strain, wear resistance, tear resistance and the like by adding nano fillers (such as white carbon black, montmorillonite, graphene, carbon nano tubes and the like). Under the service condition of the material, different external field parameters can influence the service life and the actual performance of the material, and the research on the structural evolution of the filling rubber under different external field conditions (such as a stress field and a temperature field) is beneficial to further researching the performance of the high polymer material, guiding the processing technology and constructing a prediction model of the material in the service state. The nonlinear viscoelastic behavior of filled rubbers under small strains is known as the payne effect. The views of the main influencing factors for the payne effect fall into two categories: one is due to filler-rubber interaction and the other is filler-filler interaction. At present, a great deal of research shows that the reinforcing mechanism of the filling rubber is closely related to a rubber layer which is harder than matrix rubber and is formed on the surface of the filler, namely a bonding adhesive layer, and the evolution process research of the bonding adhesive and the filler network under the action of a stress field is beneficial to further revealing the essence of the payne effect, so that the correlation between the microstructure of the material and the reinforcing performance is searched.
For the structural evolution problem of the filled rubber in the stretching process, the most suitable method is in-situ detection, the most common determination methods at present are an electron microscope and a rheological method, and the electron microscope can obtain the interaction potential between fillers in the filled rubber through in-situ experiments so as to further obtain the thickness of the bonding adhesive layer. The rheological method is an indirect method, linear or nonlinear viscoelastic behavior is researched on the strength, modulus and the like of the filler polymer composite material, the filler-rubber interaction strength is indirectly represented through modulus change, and then the bond line information is fitted, however, an electron microscope needs to carry out special treatment on a sample, is easily influenced by a complex sample preparation process and operator selectivity, and can only reflect local information of the sample under the influence of a visual field and electron penetration; the rheological method can only indirectly reflect the bonding rubber information of the filling rubber through the interaction strength of the filler and the rubber, and can not directly and comprehensively reflect the real situation of the network evolution of the filling rubber structure.
Disclosure of Invention
In view of the above, the present invention aims to provide an in-situ, fast, effective, direct, and comprehensive method for measuring evolution of a filled rubber structure network based on small-angle neutron scattering.
In order to achieve the purpose, the invention specifically adopts the following technical scheme:
a filling rubber structure network evolution measuring method based on small-angle neutron scattering is characterized by comprising the following steps:
(1) Sample preparation
Adding a filler into a rubber base material to form a rubber base body, and vulcanizing the rubber base body to obtain a vulcanized filled rubber sample to be detected;
(2) Sample installation
Confirming that the light source, the in-situ tensile sample stage and the detector are on the same straight line, and placing the filled rubber sample to be detected on the in-situ tensile sample stage with small-angle neutron scattering;
(3) In situ experiment
Respectively carrying out static small-angle neutron scattering measurement on the filled rubber sample to be measured at different distances from the sample to the detector, and then selecting a proper stretching mode to carry out in-situ stretching small-angle neutron scattering measurement to obtain static small-angle neutron scattering experimental data, in-situ stretching small-angle neutron scattering experimental data and corresponding stretching mechanical curve data of the filled rubber sample to be measured;
(4) Data processing
Respectively carrying out sector integral on static small-angle neutron scattering experimental data vertical/horizontal to the stretching direction and in-situ stretching small-angle neutron scattering experimental data in different time periods, sequentially carrying out background subtraction to obtain a static scattering curve and a dynamic scattering curve, and respectively carrying out static absolute intensity correction and dynamic relative intensity correction on the static scattering curve and the dynamic scattering curve to obtain a static absolute intensity curve and a dynamic relative intensity scattering curve; the background deduction refers to deduction of influences of the background of air scattering under the test environment on small-angle neutron scattering experimental data, the static absolute intensity correction refers to normalization correction of the ordinate of a static scattering curve, and the dynamic relative intensity correction refers to normalization correction of the ordinate of a dynamic scattering curve caused by the same thickness change of the same sample due to uniform stretching under the same test condition.
(5) Model fitting
And performing model fitting on the absolute intensity and relative intensity curves to obtain the structural network evolution condition of the filled rubber sample to be detected under the action of the stress field.
Further, the step (1) comprises the step (1.1), a deuterated chain is doped into the rubber base material, then a filler is added to obtain a rubber matrix containing the deuterated chain, and then the rubber matrix containing the deuterated chain is vulcanized to obtain a vulcanized filled rubber sample to be tested. This patent uses the small angle neutron scattering of contrast transform to realize that the bonding glue film to rubber carries out the sign.
Further, the step (3) includes a step (3.1) of confirming whether the measurement under the different distance conditions from all the samples to the detector is completed or not, if not, continuing the measurement under the distance conditions from a new sample to the detector, and if the measurement under all the conditions is completed, restoring and returning to the test site. Different distances from the sample to the detector correspond to different measurement scales, and multi-scale representation of structural evolution of the filled rubber sample to be detected is realized.
Further, in the step (3), the in-situ stretching small-angle neutron scattering measurement is performed in any one of different stretching rates and stretching temperatures. This patent uses tensile small angle neutron scattering of normal position to obtain corresponding mechanical curve when the rubber structure characterization, has carried out the characterization to its modulus.
Further, in the step (5), a suitable model is selected and fitted according to different filled rubber samples.
Further, in the step (1), the rubber substrate is any one of silicon rubber, natural rubber, styrene butadiene rubber, nitrile rubber, ethylene propylene rubber, isoprene rubber and butadiene rubber;
further, in the step (1), the filler is any one of white carbon black, montmorillonite, graphene, carbon nanotubes or MQ silicon resin.
Furthermore, the neutron source used by the neutron scattering technology can be used together with a neutron source large scientific device with multiple modes, namely any one of a reactor neutron source, a pulse reactor neutron source and a spallation neutron source can be adopted.
The invention is based on the small-angle neutron scattering technology to measure the structural evolution of the rubber, and can effectively represent the filler network structural information of the filled rubber due to the specific small-angle scattering mechanism of the small-angle neutron scattering technology and the advantage of strong neutron penetrability; combined with hydrogen/deuterium labeled contrast variation techniques to control the scattering length density of the material to characterize the desired bond gel layer structure information. And in combination with in-situ tensile detection, the scattering structure information can be obtained, and simultaneously, a corresponding mechanical curve can be obtained, so that the modulus of the scattering structure information is characterized. The in-situ small-angle neutron scattering technology can be used for effectively representing rubber in combination with rubber network and filler network evolution under the action of a stress field to construct a dynamic mechanical structure model of the rubber. The invention relates to a method for effectively clarifying the structural evolution of rubber under the action of a stress field in situ.
The filling rubber structure network evolution measuring method based on small-angle neutron scattering has the following advantages:
1. the preparation process of the filled rubber sample to be detected is simple, the filled rubber sample to be detected is not damaged, no macroscopic and microscopic structure damage or change is caused, and the method has the advantages of in-situ and rapidness.
2. The small-angle neutron scattering technology can effectively represent 1-100 nanometer structures in the material, and by combining with in-situ tensile detection, the filler network evolution condition of the filled rubber under large scale can be observed visually and dynamically, so that the method has the advantages of effectiveness and intuition.
3. The hydrogen/deuterium substitution contrast change small-angle neutron scattering is combined with in-situ tensile detection, the information of the combined glue layer of the filled rubber can be effectively and visually separated, the evolution condition of the combined glue network under the action of a stress field can be visually and dynamically observed, and the method has the advantages of effectiveness and intuition.
4. The small-angle neutron scattering is combined with in-situ tensile detection, the structural information of the filled rubber can be obtained through scattering data, and meanwhile, a corresponding mechanical curve is obtained, so that the data is further quantitatively analyzed;
5. by means of model fitting, parametric information of the structural evolution of the filling rubber can be further obtained.
The structural evolution of the filled rubber determined by the invention is an important parameter for effectively researching the mechanical response problem of the filled rubber, and can be used for further and deeply exploring the influence of the micro morphological characteristics of the filled rubber on the mechanical property of the filled rubber.
Drawings
FIG. 1 is a schematic diagram of a testing device layout of the method for measuring evolution of a filled rubber structure network based on small-angle neutron scattering according to the present invention;
FIG. 2 is a flow chart of the operation of the method for measuring the evolution of the filled rubber structure network based on small-angle neutron scattering according to the present invention;
FIG. 3 is a plot of the one-dimensional integrated small angle neutron scattering in the vertical and horizontal directions for an in-situ stretch of 2000 to 2400s for rubber sample V50H in example 1;
FIG. 4 is a plot of the one-dimensional integrated small angle neutron scattering in the vertical and horizontal directions for an in-situ stretch of 2000 to 2400s for rubber sample V50D in example 2;
in the figure, 1, a bearing table 2, an incident beam 3, a detector 4, a filled rubber sample to be detected 5, a clamp 6, a slide block 7, a force sensor 8 and a computer for controlling stretching are adopted.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
The rubber substrate of the embodiment is polymethyl vinyl siloxane, the filler is fumed silica, the small-angle neutron scattering test instrument is an Suan Ni neutron small-angle neutron scattering spectrometer of a Chinese sheep Yang research pile, the sample table is an in-situ tensile sample table, and the flow chart is shown in fig. 1, and the specific steps are as follows:
(1) Sample preparation
Adding a filler into rubber base material polymethylvinylsiloxane to form a rubber base body, and vulcanizing the rubber base body to obtain a vulcanized filled rubber sample to be tested, wherein the sample is named as V50H (V represents vulcanization, 50 represents that 50g of filler is added to every 100g of rubber base material, and H represents that no deuterated chain exists);
(2) Sample installation
Placing an in-situ tensile sample table on a scattering bearing table 1, confirming that the central axes of the sample table, a light source 2 and a detector 3 are on the same straight line, and fixing a to-be-detected filled rubber sample 4 (V50H) on the in-situ tensile sample table for small-angle neutron scattering by using a clamp 5;
(3) In situ experiment
And starting the incident beam 2 and the detector 3, respectively carrying out static small-angle neutron scattering measurement on the filled rubber sample 4 to be tested at different distances from the sample to the detector 3, then carrying out in-situ stretching small-angle neutron scattering test on the rubber sample 4 to be tested through the slide block 6 at a stretching speed of 0.5mm/min, and stopping stretching after 40min of stretching test. The force sensor 7 transmits data to the computer 8 to obtain a stress-strain mechanical curve, and the detector 3 obtains static small-angle neutron scattering experimental data and in-situ tensile small-angle neutron scattering experimental data of the filled rubber sample 4 to be detected; after the completion of the whole stretching scattering experiment and the measurement of the mechanical curve are confirmed, the incident beam 2, the detector 3 and the computer 8 for controlling stretching are closed, the sample table is dismounted from the bearing table 1, the sample 4 is dismounted from the clamp 5, whether the measurement under different distance conditions from all samples to the detector is completed or not is confirmed, if the measurement is not completed, the measurement under the distance conditions from a new sample to the detector is continued, and if the measurement under all conditions is completed, the test site is restored and returned. The different distances from the sample to the detector in the step are respectively L =10.47m, 4.25m and 1.11m under the wavelength lambda =0.53nm, and correspond to different scales required to be measured by the filled rubber sample to be measured;
(4) Data processing
Respectively carrying out sector integral on static small-angle neutron scattering experimental data of V50H vertical/horizontal to the stretching direction and in-situ stretching small-angle neutron scattering experimental data of different time periods, sequentially carrying out background subtraction to obtain a static scattering curve and a dynamic scattering curve, and respectively carrying out static absolute intensity correction and dynamic relative intensity correction on the static scattering curve and the dynamic scattering curve to obtain a static absolute intensity curve and a dynamic relative intensity scattering curve of V50H; the background deduction refers to deduction of influences of the background of air scattering under the test environment on small-angle neutron scattering experimental data, the static absolute intensity correction refers to normalization correction of the ordinate of a static scattering curve, and the dynamic relative intensity correction refers to normalization correction of the ordinate of a dynamic scattering curve caused by the same thickness change of the same sample due to uniform stretching under the same test condition.
(5) Model fitting
For the static absolute intensity curve and the dynamic relative intensity scattering curve of V50H, guinier-porod fitting is used, and the formula is shown in detail
When q is less than or equal to q 1 When the temperature of the water is higher than the set temperature,
when q is not less than q 1 When the temperature of the water is higher than the set temperature,
wherein I (q) is the absolute scattering intensity, q is the scattering vector, G is the Guinier factor, R is the absolute scattering intensity g Is the gyration radius, P is the Porod index, s is the size variable, the above numerical values are all given by a small-angle neutron scattering test instrument or obtained by the query of a standard database; and finally obtaining the structural network evolution condition of the filled rubber sample to be detected under the action of the stress field. The rubber V50H sample to be tested obtained in the embodiment is vertical and horizontalThe results show that the V50H sample has no orientation in the vertical and horizontal directions during the stretching process, and the radius of gyration of the V50H sample in the vertical and horizontal directions is the same through model fitting, that is, the aggregate is not deformed; finally, the evolution situation of the filler network under stress is obtained, namely, the filler network is not deformed along with the increase of the stress.
Example 2
This example is substantially the same as the embodiment of example 1, and is specifically different in that:
the sample preparation in the step (1) comprises the following specific steps:
doping deuterated polydimethylsiloxane into rubber substrate polymethylvinylsiloxane, then adding a filler to form a rubber substrate containing a deuterated chain, and vulcanizing the rubber substrate to obtain a vulcanized filled rubber sample to be tested, wherein the vulcanized filled rubber sample is named as V50D (V represents vulcanization, 50 represents that 50g of filler is added to every 100g of rubber substrate, and D represents that the rubber substrate contains the deuterated chain);
the one-dimensional integrated dynamic relative intensity curve of the rubber V50D sample to be tested in the vertical and horizontal directions obtained in the embodiment is shown in FIG. 4; the results show that the V50D sample has orientation in the direction perpendicular to the stretching direction, the orientation increases along with the increase of strain, and the orientation is more obvious as the q value is smaller; the evolution condition of the bonding glue layer under stress is obtained through model fitting, namely the thickness of the bonding glue along the stretching direction is increased along with the increase of the strain, and the thickness of the bonding glue perpendicular to the stretching direction is decreased along with the increase of the strain.
Table 1 shows the information table of the to-be-tested filler rubber obtained in each embodiment, and the network evolution of the bonding glue and the network evolution measurement result of the bonding glue of the to-be-tested filler rubber can be known.
TABLE 1
Claims (5)
1. A filling rubber structure network evolution measuring method based on small-angle neutron scattering is characterized by comprising the following steps:
(1) Sample preparation
Doping a deuterated chain into a rubber substrate, then adding a filler to obtain a rubber substrate containing the deuterated chain, and then vulcanizing the rubber substrate containing the deuterated chain to obtain a vulcanized filled rubber sample to be tested;
(2) Sample mounting
Confirming that the light source, the in-situ tensile sample stage and the detector are on the same straight line, and placing the filled rubber sample to be detected on the in-situ tensile sample stage with small-angle neutron scattering;
(3) In situ experiment
Respectively carrying out static small-angle neutron scattering measurement on the filled rubber sample to be measured at different distances from the sample to the detector, then selecting a proper stretching mode to carry out in-situ stretching small-angle neutron scattering measurement, and respectively obtaining static small-angle neutron scattering experimental data, in-situ stretching small-angle neutron scattering experimental data and corresponding stretching mechanical curve data of the filled rubber sample to be measured; wherein the stretching mode is any one of different stretching rates and stretching temperatures;
(4) Data processing
Respectively carrying out sector integration on static small-angle neutron scattering experimental data vertical to/horizontal to the stretching direction and in-situ stretching small-angle neutron scattering experimental data in different time periods, sequentially carrying out background subtraction to obtain a static scattering curve and a dynamic scattering curve, and respectively carrying out static absolute intensity correction and dynamic relative intensity correction on the static scattering curve and the dynamic scattering curve statically to obtain a static absolute intensity curve and a dynamic relative intensity scattering curve;
(5) Fitting of models
And performing model fitting on the absolute intensity and relative intensity curves to obtain the structural network evolution condition of the filled rubber sample to be detected under the action of the stress field.
2. The evolution determination method for the network of the filled rubber structure based on the small-angle neutron scattering according to claim 1, wherein the step (3) further comprises restoring and homing the test site after the measurement under the condition of different distances from all samples to the detector is completed.
3. The evolution measurement method for the filled rubber structure network based on the small-angle neutron scattering according to claim 1, characterized in that: in the step (1), the rubber matrix of the filled rubber sample is any one of silicon rubber, natural rubber, styrene butadiene rubber, nitrile rubber, ethylene propylene rubber, isoprene rubber and butadiene rubber.
4. The method for measuring evolution of filled rubber structure network based on small-angle neutron scattering according to claim 1, characterized in that: in the step (1), the filler is any one of white carbon black, montmorillonite, graphene, carbon nano tube or MQ silicon resin.
5. The method for measuring evolution of filled rubber structure network based on small-angle neutron scattering according to claim 1, characterized in that: in the step (3), the neutron source used for small-angle neutron scattering adopts one of a reactor neutron source, a pulse reactor neutron source and a spallation neutron source.
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