Rheological Properties and Microstructure of Printed Circuit

March 31, 2017

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Rheological Properties and Microstructure of Printed Circuit Boards Modified Asphalt

Yu Xin; Dong Fuqiang; Liang Xingmin; Ji Zezhong(College of Civil and Transportation Engineering, Hohai University, Nanjing 210098)

Abstract: The asphalt modified with different printed circuit boards (PCBs) content (0, 5%, 10%, and 15%) was prepared in this study. The general properties, rheological properties, temperature sensitivity, fatigue resistance, and morphology of the PCBs modified asphalt were investigated by conventional tests, the Brookfield viscometry tests, the dynamic shear rheometer (DSR) tests, the bending beam rheometer (BBR) tests, and the fluorescence microscopy tests. And the influence of PCBs content on the above-mentioned properties was analyzed systematically. The results showed that the addition of PCBs could improve the high temperature performance, the low temperature performance, and the temperature sensitivity property of the modified asphalt, while compromising with the fatigue resistance of the modified asphalt. With the increase of PCBs content, the modified asphalt could have better softening points, viscosity, failure temperature, and temperature sensitivity, while its low temperature performance and fatigue resistance became worse to different degree. And the particle size of PCBs became bigger and non-uniform with an increasing PCBs content. According to the above-mentioned properties, the optimum PCBs content was specified at less than 10% in the modified asphalt system.Key words: PCBs modified asphalt; viscoelasticity behavior; temperature sensitivity; fatigue resistance; morphology

1　Introduction

Nowadays, tens of thousands of tons of waste printed circuit boards (PCBs) from large household appliances such as refrigerators, personal stereos, and computers are being scrapped every year[1]. If the waste PCBs cannot be treated properly, it will pollute the local environment[2]. There are many methods to recycle the waste PCBs including landfill, incineration, thermal denaturalization, and wet chemical separation, etc.[3] Among them, the landfill is the main method to dispose of the useless components in waste PCBs. However, this approach would terribly waste the valuable resources and pollute the environment[4].According to the analysis of PCBs, besides nearly 28% of metals consisting of abundant non-ferrous metals such as Cu, Al, and Sn, the dominating components of PCBs are composed of 72% of nonmetals such as resins, plastics, polymers and fibers[5-6]. Many researches are focused on recovery of metals from the discarded PCBs[7-8]. However, how to deal with the reclamation of nonmetals from waste PCBs in an environmentally benign approach is one of the most difficult problems, so the objective of this paper

is to research the utilization of non-metals from waste PCBs.Faced with the highway overloading, high traffic volume, and climatic change, the base asphalt cannot meet the demand of asphalt mixture pavement[9-10]. Therefore, the modified asphalt such as the styrene-butadiene-styrene (SBS) modified asphalt[11], the crumb rubber modified asphalt[12], and the styrene-butadiene-rubber (SBR) modified asphalt[13], are widely used in the asphalt road pavement. And so far the above-mentioned modified asphalt can improve the high-temperature and low-temperature performance of asphalt pavement. Fortunately, there are many nonmetals such as resins, plastics, and polymers, which are similar to the components of SBS and SBR in many aspects, so the nonmetals of PCBs probably can improve the performance of base asphalt. Therefore, it is effective and economic to prepare and study the PCBs modified asphalt in a bid to realize the recycle of waste resources,

Received date: 2016-09-26; Accepted date: 2017-01-23.Corresponding Author: Dong Fuqiang, E-mail: [email protected]; Telephone: +86-13951887021.

China Petroleum Processing and Petrochemical Technology 2017, Vol. 19, No. 1, pp 72-80Scientific Research

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protect the environment, and reduce the production cost of modified asphalt.As for the PCBs modified asphalt, many researchers have found out that the PCBs modifier can improve the high temperature performance of asphalt[14-15]. However, the low temperature performance and microstructure of the PCBs modified asphalt have not been investigated yet, and whether the influence of PCBs on the performance of asphalt is similar to that of the conventional polymer modified asphalt has not been reported.The objective of this study is to investigate the influence of PCBs content on the rheological properties and microstructure of the modified asphalt. The general properties, rheological properties, temperature sensitivity, fatigue resistance, and morphology of the PCBs modified asphalt were investigated by conventional tests, the Brookfield viscosity tests, the DSR tests, the BBR tests, and the fluorescence microscopy tests. Finally, the optimum content of PCBs for the modified asphalt was obtained.

2　Materials and Experiments

2.1　Materials

The #70 asphalt from the Ssangyong Asphalt Plant of South Korea was selected as the base asphalt for preparing the PCBs modified asphalt, with its properties shown in Table 1. In this study, the nonmetal components from waste PCBs were used as a modifier to improve the performance of base asphalt, and the particle size of the PCBs powder was smaller than 0.075 mm.

Table 1　Properties of base asphalt

Items Results Test methods

Density at 15 oC, g/cm3 1.065 GB/T 8928

Penetration at 25 oC, 0.1 mm 63 GB/T 4509

Softening point, oC 45.3 GB 2294

Viscosity at 60 oC, Pa•s 317.4 ASTM D1102

Ductility at 15 oC, cm >100 ASTM D5801

Flash point, oC 345 GB/T 267

2.2　Preparation of PCBs modified asphalt samples

A FM300-digital high shear homogenizer was used to prepare the PCBs modified asphalt samples with different PCBs content (5%, 10%, and 15% by weight of base asphalt). Firstly, the base asphalt was heated to the fluid

condition, and then poured into a 1000-mL spherical flask. Then a given mass of PCBs modifier was added to the base asphalt and mixed for about 1.5 h at 165 oC at a rotation speed of 4 000 r/min. Meanwhile, the base asphalt was also treated by the same preparation process serving as the blank sample. At last, the prepared samples were used for the following tests.

2.3　Testing methods

2.3.1　Conventional properties tests

The conventional tests for the PCBs modified asphalt including the softening point, penetration, and ductility were carried out in this study. The softening point (the ring and ball test) was measured according to the Chinese standard method GB/T 4507. The penetration test was carried out at 25 oC according to the Chinese standard method GB/T 4509. And the ductility test was determined at 15 oC on the basis of the Chinese standard method GB/T 4508.

2.3.2　Rotational viscosity tests

Viscosity is an important property for evaluating the high temperature performance and workability of asphalt, so the viscosity of asphalt must be appropriate during construction process. In this study, the Brookfield viscometer tests according to standard method AASHTO T 316-04 [16] were performed for the PCBs modified asphalt at different temperatures (100 oC, 110 oC, 135 oC, 150 oC, and 160 oC).

2.3.3　Dynamic shear rheometer (DSR) test

The temperature sweep tests and frequency sweep tests were conducted using a TA-AR1500ex DSR (using 25-mm diameter parallel plates with 1 mm gap) for the non-modified and modified asphalt binders at a temperature ranging from 10 oC to 80 oC with intervals of 5 oC and at a frequency range from 0.1 rad/s to 100 rad/s, respectively. The rutting resistance factor G*/sinδ, the storage modulus (G′), the loss modulus (G″) and the fatigue resistance factor G*•sinδ were obtained from the results of tests. And then the failure temperature[17], the temperature sensitivity[18] and the fatigue temperature[19] of the non-modified and modified asphalt samples were calculated by the relationship between G*/sinδ, G′, G″, and G*•sinδ and testing temperature.

Yu Xin, et al. China Petroleum Processing and Petrochemical Technology, 2017, 19(1): 72-80

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2.3.4　Bending beam rheometer (BBR) test

The low temperature performance of the non-modified and modified asphalt with different PCBs content was determined by the BBR tests at a testing temperature of -12 oC, -18 oC, and -24 oC, respectively. And the creep stiffness (S) and m-value could be obtained to evaluate the low temperature performance of samples[20-21].

2.3.5　Morphology characterization

The morpho logy can be used to desc r ibe the microstructure interacting between the asphalt and the polymer and the compatibility of the polymer modified asphalt. And the fluorescence microscopy technique is a most valuable method to study the morphology of the polymer modified asphalt[22]. In this study, the state of PCBs dispersed in asphalt was observed by an Olympus IX83 fluorescence microscope. The samples for the morphology analysis were prepared using the preparation method suggested by Dong, et al. [11]

3　Result and Discussion

3.1　Conventional properties of asphalt

The general properties of asphalt including the softening point, the penetration at 25 oC, and the ductility at 15 oC were used to evaluate the high-temperature and low-temperature performance of asphalt in this study. The influence of different PCBs content on the conventional properties of modified asphalt was studied. It can be seen from Figure 1 that addition of PCBs modifier had a great effect on the performance of asphalt. In comparison to the base asphalt, the penetration of the modified asphalt decreased linearly with an increasing PCBs content. Therefore it can be concluded that with the increase of PCBs content the softening point of the modified asphalt samples increased, indicating that the asphalt became harder after the addition of PCBs. As for the high temperature performance of the modified asphalt, it is an advantage brought about to the base asphalt, because the asphalt with higher softening point would have less permanent deformation. Hence the higher the softening point is, the better the high temperature performance would be. The low temperature performance of the non-modified and modified asphalt with different PCBs content was

evaluated by the ductility test. As shown in Figure 1, the PCBs content had a significant effect on the ductility of the modified asphalt. With the increase of PCBs content the ductility of the modified asphalt decreased rapidly at first and then slowed down, indicating that the low temperature performance of the modified asphalt became worse as compared to the base asphalt. Although the ductility of asphalt decreased with the increase of PCBs content, the low temperature performance of the asphalt mixture containing PCBs was improved and became better[23].

Figure 1　Influence of PCBs content on the general properties of modified asphalt

■—Softening point; ●—Penetration at 25 oC;▲—Ductility at 15 oC

3.2　Viscosity-temperature property

The viscosity-temperature property is an index to evaluate the high temperature performance of the modified asphalt and the workability of asphalt mixture. The viscosity-temperature performance of the non-modified and modified asphalt with different PCBs content is presented in Figure 2. It can be seen that the viscosity of the non-modified and modified asphalt decreased with an increasing test temperature, and the PCBs content had a great influence on the viscosity of the modified asphalt within the temperature range studied.Compared to the non-modified asphalt, the addition of PCBs could improve the viscosity of asphalt. Meanwhile, with the increase of PCBs content, the viscosity of the modified asphalt also increased to different degree, and when the PCBs content increased from 10% to 15%, the viscosity of the modified asphalt showed a great change. Furthermore, the viscosity variation range of the modified asphalt with different PCBs content differed


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at all test temperatures studied, so that the lower the test temperature was, the higher the change in viscosity of the modified asphalt with different PCBs content would be. The higher viscosity indicated that the higher PCBs content in the modified asphalt showed a better effect on the high temperature performance of asphalt. And the workablity of asphalt mixture with 10 wt% of PCBs was better than that with 15 wt% of PCBs.

Figure 2　Influence of PCBs content on the viscosity-temperature property of the modified asphalt■—PCBs content is 0%; ●—PCBs content is 5.0%;▲—PCBs content is 10%; ▼—PCBs content is 15%

3.3　Viscoelasticity behaviour

As regards the polymer modified asphalt, the components and properties of polymers can have a great effect on the viscoelastic behavior of asphalt, which would impose a significant influence on the performance of asphalt pavement. And the dynamic rheological performance (storage modulus G′ and loss modulus G″) is more sensitive to the changes of components in the modified asphalt. The rheological property’s dependence on time or frequency is most important, and the frequency and temperature dependence of G′ and G″ of the non-modified and modified asphalt with different PCBs content are presented in Figure 3 and Figure 4, respectively. It can be seen from Figure 3 that the values of the storage modulus G′ and the loss modulus G″ were enhanced dramatically with an increasing frequency. And the values of G′ and G″ increased almost 104 times when the frequency changed from 0.1 to 100 rad/s. As for the non-modified asphalt, the value of the loss modulus G″ was higher than that of the storage modulus G′, suggesting that the viscous component had surpassed the elastic component. And with the increase of PCBs content, the

storage modulus G′ and the loss modulus G″ all increased too. Meanwhile, the variation range of the loss modulus G″ was bigger than that of the storage modulus G′, indicating that the loss modulus G″ was more sensitive to frequency than the storage modulus G′[24]. A higher storage modulus G′ suggested that the addition of PCBs could increase the elastic component in the modified asphalt, and a higher storage modulus G″ could be favorable to the high temperature performance of asphalt.As shown in Figure 4, with the increase of test temperature, the values of the storage modulus G′ and the loss modulus G″ decreased by 104 times. And being similar to the results of frequency sweep test, the value of the loss modulus G″ was higher than that of the storage modulus G′. However, the variation range of storage modulus G′ was bigger than that of the loss modulus G″ with the increase of PCBs content, suggesting that the addition of PCBs could increase the elastic component in the modified asphalt.Furthermore, the rutting resistance factor G*/sinδ could be obtained from the temperature sweep tests to evaluate the high temperature performance of asphalt. And the factor G*/sinδ of the non-modified and modified asphalt with different PCBs content is illustrated in Figure 5. It can be learned that the rutting resistance factor increased gradually with an increasing PCBs content, which was consistent with the trend dependence on PCBs contents referred to in the literature[15].In order to evaluate accurately the high temperature performance of the PCBs modified asphalt, the failure temperature was selected. Here the failure temperature is a temperature when the rutting resistance factor G*/sinδ is identified at 1.0 kPa. The failure temperature of the non-modified and modified asphalt with different PCBs content can be obtained from Figure 5 and is presented in Table 2. It can be found out that the PCBs content had a great influence on the failure temperature of the modified asphalt. In comparison to the non-modified asphalt, the addition of PCBs modifier could improve the failure temperature performance of asphalt. Meanwhile, as the PCBs content increased, the failure temperature of modified asphalt also increased to some extent. To be specific, there was a great improvement of failure temperature when the PCBs content increased from 10%


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to 15%. In a word, the PCBs modified asphalt showed a higher permanent deformation resistance than the non-modified asphalt, which was consistent with the above-mentioned results.

Table 2　The failure temperature of modified asphalt with different PCBs content

PCBs content, % Failure temperature, oC

0 67.65

5.0 69.5610.0 69.67

15.0 72.15

3.4　Temperature sensitive property

The temperature sensitive property of asphalt plays an important role in the road service performance of asphalt pavement. And many researchers[25] have found out that a better temperature sensitivity is favorable to the resistance of asphalt to the low temperature cracking and the high temperature deformation. It can be concluded from the statement in Section 3.3 that the storage modulus G′ and the loss modulus G″ are sensitive to temperature. Therefore, the variations in relationship between the storage modulus G′ and the temperature, as well as between the loss modulus G″ and the temperature were used to evaluate the temperature sensitivity of the modified asphalt as illustrated in Figure 6.

Figure 6　Logarithm of storage modulus and loss modulus■—PCBs content is 0%; ●—PCBs content is 5.0%;▲—PCBs content is 10%; ▼—PCBs content is 15%

Figure 5　Influence of PCBs content on the G*/sinδ of modified asphalt

■—PCBs content is 0%; ●—PCBs content is 5.0%;▲—PCBs content is 10%; ▼—PCBs content is 15%

Figure 3　Frequency dependence of G′ and G″ of modified asphalt with different PCBs content at 60 oC


Figure 4　Temperatures dependence of G′ and G″ of modified asphalt with different PCBs content■—PCBs content is 0%; ●—PCBs content is 5.0%;▲—PCBs content is 10%; ▼—PCBs content is 15%

It can be seen from Figure 6 that the relationship between lgG′ and lgT and the relationship between lgG″ and lgT showed a better linearity. And the statistical linear regression equations for these relationships could be obtained. Furthermore, the slopes and absolute values of each regression line were calculated, with the results listed in Table 3. Some researchers[26] have found that the lower the value of slope is, the better the temperature sensitivity would be. As listed in Table 3, in comparison to the non-modified asphalt, the value of slopes showed a


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great drop, indicating that PCBs could improve the temperature sensitivity of asphalt evidently. Meanwhile, with the increase in PCBs content, the value of slopes

decreased slightly. It can be indicated that the higher the PCBs content is, the better the temperature sensitivity of modified asphalt would be.

Table 3　Absolute slope values for the regression lines in Figure 6

PCBs content, %Absolute slope value for lgG′ regression

equationAbsolute slope value for lgG″ regression

equation

0 59.470 8 43.569 9

5.0 55.773 6 41.923 7

10.0 54.166 9 41.698 8

15.0 53.271 8 41.347 7

3.5　Fatigue resistance

It can be suggested that the fatigue resistance performance of asphalt binder has a significant influence on the service life of asphalt pavement[27]. To evaluate the fatigue resistance of the non-modified and modified asphalt with different PCBs content, the RTFOT tests and PAV tests were conducted. And then the fatigue resistance factor G*•sinδ were obtained from the DSR tests in a temperature range from 10 oC to 50 oC with an interval of 5 oC. And the relationship between lgG*•sinδ and the temperature is illustrated in Figure 7.According to the literature report[19], a lower fatigue resistance factor G*•sinδ means a better fatigue resistance. As shown in Figure 7, in comparison to the non-modified asphalt, the fatigue resistance factor G*•sinδ of the modified asphalt became higher, indicating that the PCBs modifier had unfavorable effects on the fatigue resistance of asphalt. Meanwhile, with the increase of PCBs content, the fatigue resistance factor G*•sinδ of the modified asphalt increased, and when the PCBs content increased higher, the modified asphalt became more sensitive to fatigue cracking. In order to quantify the influence of PCBs content on the fatigue resistance of the modified asphalt, the fatigue temperature, which is a temperature when the fatigue resistance factor G*•sinδ is at 5 000 kPa, has been selected and listed in Table 4. It can be seen that the fatigue temperature of the modified asphalt is higher than that of the non-modified asphalt. With the increase of PCBs content, the fatigue temperature of modified asphalt shows an increase trend too. It can be indicated that the PCBs modifier can compromise with the fatigue

performance of asphalt. However, the variation of fatigue temperature presents a significant difference as the PCBs content increases. There is a big change in fatigue temperature when the PCBs content increases from 10% to 15%. In respect of the fatigue resistance, the optimum PCBs content should be less than 10%.

Figure 7　Temperature dependence of G*·sinδ of modified asphalt with different PCBs content


Table 4　Ultimate fatigue temperature of modified asphalt with different PCBs content

PCBs content, % Ultimate fatigue temperature, oC

0 10.87

5.0 12.28

10.0 12.77

15.0 34.01

3.6　Creep stiffness and the m-value

The low temperature performance of the non-modified and modified asphalt was evaluated by the BBR tests. And the creep stiffness and m-value were determined for samples at the test temperature of -12 oC, -18 oC and


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-24 oC that corresponded to the field temperature of -22 oC, -28 oC and -34 oC, respectively. According to the standard method AASHTO T313-04[28], the maximum stiffness and minimum m-value meeting the low temperature asphalt binder grade should be 300 MPa and 0.3, respectively.The stiffness and m-values of the non-modified and modified asphalt with different PCBs content are presented in Figure 8. On the whole, the PCBs content has a great effect on the low temperature performance of the modified asphalt. Compared to the non-modified asphalt, PCBs can decrease the stiffness and increase the m-value, indicating that the PCBs modifier can enhance the low temperature performance of asphalt. However, with the increase of PCBs content, the stiffness increases and the m-value decreases, which means that the low temperature performance of the modified asphalt becomes worse.As for the non-modified asphalt, the stiffness and m-value can meet the specification for -28 oC and -22 oC. After adding the PCBs modifier, the low temperature performance becomes better, and when the PCBs content is equal to 5.0% and 10%, the low temperature performance of the modified asphalt can meet the specifications for the field temperature of -34 oC, -28 oC and -22 oC. However, when the PCBs content increases to 15%, the low temperature performance cannot meet the specification demand for -34 oC. In a word, when the PCBs content is less than 10%, the low temperature performance of the modified asphalt is better than that of the non-modified asphalt.

4　Morphology

In order to understand the microstructure of the PCBs modified asphalt, especially the state of dispersion of PCBs in the asphalt, the morphology was studied by a fluorescence microscope. Figure 9 presents the morphology change of the modified asphalt with different PCBs content.As shown in Figure 9, it can be found out that the phase morphology was converted from one phase to a continuous asphalt phase with dispersed PCBs phase after adding the PCBs modifier, and the PCBs content had a great effect on the particle size of PCBs phase. With the increase of PCBs content, the particle size of PCBs became bigger and non-uniform. Specifically, when the PCBs contents were 5% and 10%, the particle size of PCBs in asphalt was small and uniform, while the particle size became larger and irregular when the PCBs content in asphalt reached 15%. Meanwhile, the dimensional network did not appear, denoting that there was no chemical reaction between the PCBs modifier and the asphalt[29-30]. In addition, due to the limitation of saturates and aromatic components in the base asphalt, when the PCBs content was too higher, the particle size of PCBs thereby became bigger and non-uniform.

5　Conclusions

The general properties, rheological properties, temperature sensitivity, fatigue resistance, and morphology of

Figure 8　Stiffness and m-value of PCBs modified asphalt at different temperatures

—12 oC; —18 oC; —24 oC;

Figure 9　The morphology of modified asphalt with different PCBs content (×200)


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the PCBs modified asphalt were investigated by the conventional tests, the Brookfield viscosity tests, the DSR tests, the BBR tests, and the fluorescence microscopy tests. And the influence of PCBs content on the above-mentioned properties was analyzed systematically.Compared to the non-modified asphalt, the addition of PCBs could improve the high temperature performance, the low temperature performance, and the temperature sensitivity property of the modified asphalt. With the increase of PCBs content, the modified asphalt could possess better softening point, viscosity, failure temperature, and temperature sensitivity, while its low temperature performance became worse.Adding PCBs modifier could compromise with the fatigue resistance of asphalt. With the increase of PCBs content, the fatigue resistance of the modified asphalt decreased to different degree. And the particle size of PCBs became bigger and non-uniform when the PCBs content continued to increase. Upon taking the above-mentioned properties into consideration, the optimum PCBs content should be less than 10 wt% in the modified asphalt system.

Acknowledgments: This work was funded by the Natural

Science Foundation of Jiangsu Province for Distinguished

Young Scholars (BK20150038), the Fundamental Research

Funds for the Central Universities (2015B21614), and the China

Postdoctoral Science Foundation (2016M591759). The authors

gratefully acknowledge their financial support.

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Rheological Properties and Microstructure of Printed Circuit