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Fabrication of Nanopatterns on Silicon Surface by Combining AFM-Based Scratching and RIE Methods

  • Yanquan Geng
  • Yongda Yan
  • Jiqiang Wang
  • Yun Zhuang
Original Articles
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Abstract

This study presents an atomic force microscope (AFM)-based scratching combined with reactive ion etching (RIE) method to fabricate nanopatterns on the silicon surface. All AFM-based scratching processes are performed on the polymethylmethacrylate (PMMA) film to create features in order to protect the AFM tip from wearing and enlarge its life time. Two types of resist films are selected for the RIE process. One is only PMMA thin-film resist, and the other one contains two-layer thin-film resist which are PMMA and aluminum thin films. The nanopatterns on the silicon after etching using RIE with these two types of resist film are compared. Results show that when using PMMA film, the width of the nanopattern on silicon is larger than on the PMMA film, and the material pile-ups formed during the scratching process cannot be considered as a resist. On the contrary, the aluminum thin films can improve the quality of the transfer. It indicates that the thin-film resist with bilayers can guarantee the transfer accuracy of the features, which can expand the application of the AFM tip-based scratching technique.

Keywords

Atomic force microscopy Reactive ion etching Scratching Nanopattern 

1 Introduction

With the rapid development of nanotechnology, nanostructures have been used in various fields, especially on the silicon- and carbon-based materials [1, 2, 3, 4]. Nowadays, there are several nanofabrication approaches to create nanostructures on the silicon or carbon-based materials, such as electron beam lithography (EBL) [5], focused ion beam (FIB) lithography [6], and electrochemical machining [7]. However, the disadvantages of low throughput, complex operation and/or cost of implementation greatly hinder the development of these nanofabrication techniques.

Since atomic force microscopy (AFM) was invented in 1986 by Binning et al. [8], it has been considered as a nanoscale profilometer. When the interaction force between the tip and the sample is enlarged, the AFM tip can serve as a small cutting tool to fabricate nanostructures on the sample surface [9]. Nanogrooves, two-dimensional and even three-dimensional nanostructures, were fabricated on various material successfully, including metal, polymer and semiconductor materials [10]. Because of the low hardness of the polymer material, the silicon tip is always selected to conduct nanoscratching process [11, 12, 13]. For the metal and semiconductor materials, the diamond tip with a large stiffness cantilever is usually chosen as the cutting tool [14, 15]. However, the tip wear is the main problem when implementing long-distance scratching test, especially for machining on the semiconductor materials [15]. Thus, some scholars utilized the AFM tip first to scratch on a resist thin-film surface, and then transferred the patterns to the materials with large hardness, such as silicon or quartz, by wet etching or reactive ion etching (RIE) process [16, 17, 18, 19]. For the wet etching process, no specific equipment is needed and this method is easy to use [16, 17]. However, the dimensions of the fabricated structure are difficult to be controlled, and the transverse etching effect can lead to reducing the transfer accuracy. For the RIE process, the dimension of the etched patterns can be accurately controlled by the etching time, especially for the nanoscale desired depth. Peng et al. [20] used a diamond AFM tip to scratch on the aluminum thin-film resist directly due to the large hardness of the metal material as mentioned above. However, the large radius of the diamond tip can enlarge the width of the machined groove on the aluminum resist, which will result in low machining accuracy. Zhang et al. utilized high-rate tunable ultrasonic force nanomachining process to scratch on the PMMA/aluminum bilayers thin-film resist following RIE process to create nanogrooves on silicon substrate [18]. Because of the low hardness, the tip wear is relatively small when first scratching on the PMMA thin-film resist, even for the silicon tip. However, the difference between the influence of the single and bilayers resists on the etching results and the effect of the thickness of the resist are rarely studied.

Therefore, in the present study, an AFM tip-based scratching combined with RIE method is used to fabricate nanopatterns on silicon surface. Two types of resist films are selected for the RIE process, including PMMA and PMMA/aluminum thin-film resists. The influence of thickness of the PMMA thin film on the etched results is studied. In addition, experiments are conducted to compare the two types of thin-film resists on the etching results.

2 Experimental Detail

In this study, a commercial AFM system (Dimension Icon, Bruker Company, Germany) is employed for all nanoscratching processes. All scratching tests and measurement processes are conducted with single crystal silicon tips (TESPA, Bruker Company, Germany). The radius of the new tip is approximately 10 nm, which is evaluated by the blind reconstruction method using a titanium roughness sample (RS-15M, Bruker Company, Germany) [21]. The force constant of the cantilever is 36.5 N/m, which is calibrated according to the vibration spectrum of the cantilever presented by Sader [22].

Two types of resist films are selected for the RIE process. For the thin-film resist only containing PMMA, four thin films with different thicknesses are selected, including 10 nm, 25 nm, 48 nm and 120 nm. PMMA (Mw = 100,000 from Aladdin as 1, 2, 4 and 6% dilution in anisole) thin films are obtained by spin-coating on a cleaned silicon substrate for 50 s at 7000 rpm and baked at 160° for 20 min to increase the adhesion of the interface between films and substrates. A single crystal silicon tip is employed to scratch directly on the PMMA thin-film surface. Then, RIE process is used to transfer the features of the PMMA thin film on to the surface of the silicon substrate. In the measurement process, a new silicon tip is used in tapping mode for all image processes.

For the bilayers thin-film resist, as shown in Fig. 1, a 40-nm-thick aluminum film is first deposited on the cleaned silicon substrate surface, which accomplished by electron beam deposited method. Then, a 48-nm-thick PMMA thin film is spin-coated on the aluminum layer (Fig. 1a, b). A single crystal tip is employed to scratch directly on the PMMA thin-film surface to obtain nanogrooves (see Fig. 1c). After scratch, the sample is immersed in aqueous solution containing phosphoric acid for 50 s to transfer the nanopatterns onto the surface of the aluminum layer, as shown in Fig. 1d. In this wet etching process, the PMMA thin film is considered as a resist for the aluminum layer. Then, the sample is soaked in acetone solution to remove the PMMA thin film. Thus, the sample with only the aluminum layer can be obtained (see Fig. 1e). In the following RIE process, the aluminum layer is considered as a resist and the nanopatterns on the aluminum layer are transferred to the surface of the silicon substrate, as shown in Fig. 1f. Finally, the sample is washed in phosphoric acid solution to remove the aluminum layer and the nanopatterns on the surface of silicon are achieved.
Fig. 1

Two layers thin-film resist fabrication sequences. a 40-nm-thick aluminum deposition on cleaned silicon substrate; b 48-nm-thick PMMA spin-coated on aluminum layer; c scratching nanopatterns on PMMA layer and etching PMMA in O2 plasma till aluminum layer surface exposed; d wet etching aluminum to silicon substrate; e remove PMMA layer; f silicon etching using RIE; g remove aluminum layer and sample surface cleaning

From previous studies, in the dry anisotropic etching process, SF6/O2 gas mixtures were found to anisotropically etch silicon [23, 24]. Some researchers also found that the addition of CHF3 to the SF6/O2 plasma produced smooth etch surfaces. In the case of the aluminum layer considered as a resist in the RIE process, this resist could not react with the etch gas and the ion bombardment has little influence on the surface of this resist. Thus, SF6/O2/CHF3 gas mixtures are selected as the etching gas for the aluminum layer resist. However, for the PMMA thin-film resist, oxygen plasma can react with the PMMA thin-film material. Moreover, the surface of the PMMA thin film can be bombarded by CF x + which is introduced by CHF3. This can result in a relatively low etch selectivity. Thus, when using PMMA thin film as a resist, only SF6 is chosen as the etching gas.

In this study, the etching parameters for single- and bilayers in the RIE process are shown in Table 1. After the etching process, the thickness of the PMMA thin film used in Test 1 is reduced from 48 to 17 nm, which indicates no over etching. The etched sample is then washed ultrasonically in acetone and alcohol solutions, respectively, to remove the residual PMMA thin film. The roughness (Ra) of the substrate surface is evaluated as 0.7 nm by scanning with tapping mode of the AFM system in the range of 20 µm × 20 µm. For the aluminum layer selected in Test 2, the thickness is almost unchanged during the etching process, which is about 40 nm. The sample is first immersed in concentrated sulfuric acid and phosphoric acid for 5 min, respectively, and then washed ultrasonically in acetone and alcohol solutions, respectively. The roughness (Ra) of the substrate surface can be measured as 0.8 nm. This indicates the quality of the substrate without over etching is similar with the original surface.
Table 1

Etching parameters selected in RIE process

Test

Resist material

Etching gas

Power (W)

Pressure (Pa)

Flow (sccm)

Time (s)

1

PMMA

SF6

50

4.8

30

15

2

Al/PMMA

SF6/O2/CHF3

100

7

30/12/10

15

3 Results and Discussion

3.1 Effect of the PMMA Thin-Film Thickness on the Etched Grooves

In the RIE etching process, the etching ratio of the PMMA thin film is a critical parameter which is related to the thickness of the PMMA thin film. In order to investigate the effect of the thickness of the PMMA thin film on the etching ratio, the samples with four thicknesses of the PMMA thin film are selected, namely of 10 nm, 25 nm, 48 nm and 120 nm. In this section, the etching time is set as 50 s to over etch all the resist films. The power, pressure and flow are set to 100 W, 7 Pa and 50 sccm, respectively. After the etching process, the obtained surface of the silicon substrate is scanned by the tapping mode of AFM employing a new silicon tip to estimate the etching quality. From the measured 20 μm × 20 μm AFM images of the etched surfaces, the obtained values of the roughness Ra corresponding to the etching parameters mentioned above are 4.3 nm, 5.1 nm, 4.8 nm and 5.4 nm, respectively. This indicates that the silicon surfaces obtained by different etching parameters display similar quality and these values of Ra are much larger than the polished silicon surface before etching (less than 1 nm). The possible reason for this is explained as follows. For relatively time-consuming etching process, the raise of sample temperature results in softening the thin-film. Thus, the decrease in the thin-film thickness may be inconsistent in different ranges of the resist surface when processing under the action of ion physical bombardment. This may lead to some ranges of the resist being etched completely but other ranges of the resist still remaining on the substrate, which could enlarge the roughness of the etched silicon surface. It can also be observed that the values of Ra obtained with different thicknesses of the resist are similar. It can thus be concluded that there is little influence of the thickness of the resist on the etching quality with the over etching condition.

In this section, normal loads in the range from 7 to 10 μN are selected to scratch through the resist thin-film with different thicknesses. Figure 2a, b shows the AFM images and the corresponding cross sections of the obtained grooves on the PMMA thin film with the thickness of 10 nm and the corresponding etched groove on the silicon substrate. As shown in Fig. 2a, the width of the groove is about 290 nm, which is much larger than the radius of the AFM tip. The possible reason can be explained as follows. Owing to the PMMA solution volatilization during the spin-coating process, the stress can be generated between the resist thin-film and the silicon substrate. Moreover, the silicon substrate is hydrophobic, which can result in a relatively large stress between the resist thin-film and the silicon substrate. Thus, once the AFM tip draw through the thin-film, the material at the bottom of the groove could be teared by the stress mentioned above and a flat surface can be formed, which is much larger than the radius of the AFM tip, as shown in Fig. 3. It can be seen from Fig. 2b, the width of the groove is enlarged to 600 nm after RIE etching process. The isotropy of the RIE etching process is the possible reason. The depth of the etched groove is around 35 nm. In addition, due to the long time of the over etching process, the roughness of the silicon substrate is enlarged obviously.
Fig. 2

AFM images of the scratched groove on the PMMA thin film with the thickness of 10 nm (a) and the corresponding etched groove on the silicon substrate (b)

Fig. 3

Schematic of the width of the groove enlarged after scratching by sharp AFM tip

Figure 4a shows the groove machined on the PMMA thin film with the thickness of 25 nm, and Fig. 4b represents the corresponding etched groove on the silicon substrate. The width of the groove bottom is around 230 nm, which is also relatively large. After etching, the width of the groove bottom is enlarged to 800 nm approximately, and is inconsistent at different locations of the groove. The depth of the etched groove reaches to around 110 nm, which is much larger than that obtained by etching the thin film with the thickness of 10 nm.
Fig. 4

AFM images of the scratched groove on the PMMA thin film with the thickness of 25 nm (a) and the corresponding etched groove on the silicon substrate (b)

Figure 5 shows the grooves before and after the etching process conducted on the PMMA thin film with the thickness of 48 nm. The width of the groove bottom on the PMMA thin film is about 100 nm, and it increases to around 600 nm after the etching process. This also results from the over etching process. From the cross sections at three different locations shown in Fig. 5b, it can be found that the profiles of the groove show good consistency. The depth of the etched groove is about 220 nm, which is twice as much as that obtained by etching the thin film with the thickness of 25 nm. For the thin film with the thickness of 120 nm, the groove is not continuous with some “pitch points,” as shown in Fig. 6a, which may be caused by the stick-slip behavior of the polymer material [25]. Figure 6b, c shows the AFM and SEM images of the etched groove, respectively. It can be observed that the “pitch points” are enlarged by the etching process, which is caused by the lateral effect of the etching process.
Fig. 5

AFM images of the scratched groove on the PMMA thin film with the thickness of 48 nm (a) and the corresponding etched groove on the silicon substrate (b)

Fig. 6

AFM images of the scratched grooves on the PMMA thin film with the thickness of 120 nm (a) and the corresponding etched grooves on the silicon substrate (b), SEM image of the etched grooves (c)

In this study, the etch selectivity is defined as the ratio between the thickness of the thin film to the depth of the etched groove on the substrate. Thus, the etch selectivity for the PMMA thin films with the thicknesses of 10 nm, 25 nm, 48 nm and 120 nm can be obtained as 4.4, 4.8, 5.6 and 5.8, respectively. It can be concluded that the larger the thickness of the thin film, the higher of the etch selectivity. The thin film with relatively small thickness (10 nm and 25 nm) can be easily over etched resulting in exposing the substrate in the reaction gas, which can enlarge the roughness of the substrate compared with the original surface. While, for the thin film with relatively large thickness (120 nm), it is difficult to be cut through and the stick-slip behavior occurring during the scratching process can lead to low etching quality. Therefore, a moderate thickness of the thin film is required in the tip-based scratching and RIE combination approach, which is chosen as 48 nm in this study. Furthermore, it can be observed from the AFM images of the scratched grooves on the PMMA thin films that there are some materials accumulated on both sides of the grooves. However, there is no pile-up structure on the sides of the grooves obtained by the RIE over etching process. The possible reason can be explained as follows. The molecular chains of the PMMA thin film can be cut off by the AFM tip to form the material pile-up [26]. The etching resistance for the material pile-up may be much weaker than the original PMMA surface, which disappears by ion cluster bombardment with relatively higher energy. Thus, the material pile-up in this study cannot work as a resist to protect the substrate.

3.2 Fabrication of Nanostructures by RIE Process with One Layer Thin-Film Resist

For the single layer thin-film, we choose PMMA thin film with the thickness of 48 nm as the resist used in the RIE process. In order to scratch through the thin-film, a normal load of 7 µN is selected and the scratching velocity is set as 3 µm/s. The length of each scratch is 20 µm. The AFM image of the scratched grooves is shown in Fig. 7a. It can be found that the machined depths of the grooves are all around 50 nm, which are close to the thickness of the PMMA thin film. However, there are some intermittent material pile-ups adhered on both sides of the grooves. For the subsequent etching process, the parameters are adopted according to Table 1. The AFM image of the etched grooves is shown in Fig. 7b. The depths of the grooves are enlarged to around 170 nm, which shows good etching selectivity. Moreover, the surface of the substrate shows good quality, and the widths of the grooves are around 200 nm, which are much smaller than that obtained in Fig. 5b. These result from no over etching occurring using the parameters shown in Table 1. However, the grooves show poor uniformity for the widths at different locations along the length direction. The possible reason is the low etching resistance of the intermittent material pile-ups adhered on the sides of the groove, which can result in poor protective capability for the desired structure.
Fig. 7

AFM images of the scratched grooves on the single PMMA thin film with the thickness of 48 nm (a) and the corresponding etched grooves on the silicon substrate (b)

We also fabricate circle patterns on the PMMA thin film with a normal load of 7 µN shown in Fig. 8a. The radii for the scratched circles are 1 µm, 2 µm, 3 µm, 4 µm and 5 µm. Due to the influence of the asymmetrical geometry and the variation in scratching directions during the machining of circle feature, the machined depths show great difference from 10 nm to around 50 nm, as shown in Fig. 8a. This indicates that the PMMA thin film cannot be cut through at some locations. In particular, the machined depth of the upper half part of the circle is smaller. In the following etching process, the same parameters shown in Table 1 are selected. Figure 8b shows the AFM image of the etched circle patterns. It can be found from the horizontal and vertical cross sections of the AFM image that the etched depths of the upper half part of the circles are less than those of lower half part. In some areas, the depth depths are closed to zero. The reason can be explained as the PMMA thin film still existing after the etching process corresponding to the areas with small scratched depths. Figure 9a shows the AFM image of the circle arrays scratched on the PMMA thin films, and the radius of the circle is set as 1 µm. The machined depth also presents inconsistent along one circle scratching path, which agrees well with the machining results shown in Fig. 8a. Figure 9b shows AFM image of the corresponding etched circle arrays, and the depths show great difference from close to 0 nm to around 180 nm in the horizontal and vertical cross sections of the AFM image. Thus, it can be concluded that the AFM tip-based single scratch approach is not suitable to create grooves and circle patterns on the silicon substrate through RIE process with single layer thin-film resist.
Fig. 8

AFM images of the scratched circle patterns on the PMMA thin film with the radii of 1 µm, 2 µm, 3 µm, 4 µm and 5 µm (a), and the corresponding etched circle patterns on the silicon substrate (b)

Fig. 9

AFM images of the scratched circle arrays on the PMMA thin film (a), and the corresponding etched circle patterns on the silicon substrate (b)

3.3 Fabrication of Nanostructures by RIE Process with Bilayers Thin-Film Resist

For the bilayers thin-film resist, the thicknesses of the PMMA and aluminum thin films are also selected as 48 nm and 40 nm, respectively. The normal load is also set to about 7 μN to cut through the PMMA thin film. Figure 10a shows the AFM image of the grooves scratched on the PMMA thin film. It can be found that the profiles of the grooves are different from those shown in Fig. 7a. The possible reason can be explained as the influence of the substrate material on the PMMA thin film. It can be also observed that there are intermittent material pile-ups accumulated on the sides of the grooves. In order to transfer the nanoscale grooves onto the aluminum thin-film, the sample should be immersed in the phosphoric acid, and the steeping time should be controlled strictly according to the thickness of the aluminum thin-film. Because if the time is not enough, the thin-film cannot be etched through, conversely, if the steeping time is too long, the lateral dimension of the groove could be enlarged. In this study, for the aluminum thin-film with the thickness of 40 nm, the steeping time in the phosphoric acid is advisable to be controlled as 50 s. Figure 10b shows the AFM image of the grooves transferred on to the aluminum thin-film, and Fig. 10d shows the corresponding cross-section of the grooves. It can be seen that the quality of the transferred grooves on the aluminum thin-film are good, which indicates that the material pile-ups on the PMMA thin film almost have no influence on the transferred grooves. The grooves etched for 15 s on the silicon substrate can be observed clearly in Fig. 10c. This indicates the aluminum thin-film can be etched through after immersing in the phosphoric acid for 50 s. However, it can be observed from Fig. 10d that the measured depth of the grooves on the aluminum thin-film is only around 25 nm, which is much smaller than the thickness of the aluminum thin-film. This phenomenon results from the large ratio between the scanning size and the width of the etched grooves, and the sampling points are not enough for one groove. The same phenomenon can be found in Fig. 10e. It can be observed that the etched depths differ in the range from 70 to 100 nm. However, we select No. 3, 6 and 9 grooves in Fig. 10e to zoom in scanning with the range of 1 μm × 1 μm. The AFM images and corresponding cross sections of the selected grooves are shown in Fig. 11. It can be seen that the depths of the grooves are closed to each other, which are about 160 nm. The widths of grooves at the bottom are around 40 nm.
Fig. 10

AFM images of the scratched nanogrooves on the PMMA thin film (a), the transferred grooves on the aluminum thin-film (b), and the corresponding etched patterns on the silicon substrate (c). The cross sections of the transferred grooves on the aluminum thin-film (d) and the etched grooves on the silicon substrate

Fig. 11

AFM images and corresponding cross sections of the selected grooves (No. 3, 6 and 9) in Fig. 10e

In the previous section, the machined depths show great difference when scratching a circle pattern on the PMMA resist. In order to overcome this issue, we select the vibration-assisted scratching method to scratch on the PMMA thin film. The detail for the vibration-assisted scratching method was described in Ref. [27]. In the vibration-assisted scratching method, the normal load is set to 1.3 µN. The z vibration is excited with a frequency of 1.6 MHz, and the voltage of the excitation signal is chosen as 10 V. For the following RIE process, the etching time is select as about 4 s. Figure 12 shows the AFM images of the circle patterns scratched on the PMMA thin film and the etched grooves on the silicon substrate. It can be seen that large material pile-ups accumulated on the PMMA thin film. However, there is no influence of the material pile-ups on the etched grooves, as shown in Fig. 12b. The etched depths of the circle patterns are mainly in the range from 15 to 30 nm, and all of the depths are larger than 10 nm. This indicates that the machined depths of the circle patterns are more consistent than those shown in Fig. 9b. It indicates that the combination of the vibration-assisted scratching method and the RIE process with bilayer resist is more suitable to fabricate circle patterns on the silicon substrate.
Fig. 12

AFM images of the scratched circle arrays on the PMMA thin film (a), and the corresponding etched circle patterns on the silicon substrate (b)

4 Conclusions

In the present study, an AFM tip-based scratching combined with RIE approach is employed to fabricate nanopatterns on silicon surface. Two types of resist films are chosen for the RIE process. The silicon tip is used for all scratching operations. The following conclusions can be obtained from this study.
  1. 1.

    The effect of the thickness of the resist thin-film on the etching results is studied in detail. The widths of the etched grooves can be greatly enlarged when utilizing PMMA thin films with the thicknesses of 10 nm and 25 nm as the resists. A relatively large stress between the resist thin-film and the silicon substrate may be the possible reason. For the thickness of 120 nm, the stick-slip behavior of the polymer material leads to discontinuous grooves, while, for the thickness of 48 nm, the increase of the groove width is much smaller than those obtained by the resists with the thicknesses of 10 nm and 25 nm, which shows the best etching result.

     
  2. 2.

    For the single layer resist, the PMMA thin film with the thickness of 48 nm is chosen as the resist. The etched grooves show poor uniformity for the widths at different locations along the length direction. The low etching resistance of the intermittent material pile-ups adhered on the sides of the groove may be the possible reason. In addition, the depths of etched circle arrays show great difference at different locations, which results from the effect of the change in scratching direction when machining circle patterns.

     
  3. 3.

    For the bilayers thin-film resist, the thicknesses of the PMMA and aluminum thin films are selected as 48 nm and 40 nm, respectively. The depths and widths of the etched grooves show good consistency. In order to overcome the effect of the machined depth difference caused by the various scratching directions, the vibration-assisted scratching method is used to scratch circle patterns on the PMMA thin film, and better etching results are obtained. Moreover, experiment results indicate that the double resist layer approach is the preferred technique to overcome the negative effect of the pile-ups introduced during the scratching process.

     

The throughput of the AFM scratching combining RIE approach to fabricate nanostructure on the semiconductor materials mainly depends on the efficiency of the AFM machining process. The scratching velocity selected in this study is set as 3 µm/s, which is relatively low. However, if we use the piezoelectric actuator-based AFM tip-based high-speed machining system proposed by the authors in Ref. (25) in the further work, the theoretical cutting speed over 5 m/min can be achieved, which will enhance the throughput of the method presented in this study.

Notes

Acknowledgements

The authors gratefully acknowledge the financial supports of the National Natural Science Foundation of China (51705104, 51675134), the Foundation for Innovative Research Groups of the National Natural Science Foundation of China (51521003), Key Laboratory of Micro-systems and Micro-structures Manufacturing of Ministry of Education (Harbin Institute of Technology No. 2017KM005), China Postdoctoral Science Foundation (No. 2017M610206 and 2018T110289) and the National Program for Support of Top-notch Young Professors.

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Copyright information

© International Society for Nanomanufacturing and Tianjin University and Springer Nature 2018

Authors and Affiliations

  1. 1.Key Laboratory of Micro-systems and Micro-structures Manufacturing of Ministry of EducationHarbin Institute of TechnologyHarbinPeople’s Republic of China
  2. 2.Center for Precision EngineeringHarbin Institute of TechnologyHarbinPeople’s Republic of China

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