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Interface Components: Nanoparticles, Colloids, Emulsions, Surfactants, Proteins, Polymers
Formation and Stability of Bulk Nanobubbles in Different Solutions Shuo Ke, Wei Xiao, Nannan Quan, Yaming Dong, Lijuan Zhang, and Jun Hu Langmuir, Just Accepted Manuscript • Publication Date (Web): 26 Mar 2019 Downloaded from http://pubs.acs.org on March 27, 2019
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Formation and Stability of Bulk Nanobubbles in Different Solutions Shuo Ke,†ac Wei Xiao, †ab Nannan Quan, ac Yaming Dong, *c Lijuan Zhang, *ad and Jun Hu *ad a Shanghai
Synchrotron Radiation Facility, Shanghai Advanced Research Institute, Chinese Academy
of Sciences, Shanghai 201204, China. b School
of Resources Engineering, Xi'an University of Architecture and Technology, Xi'an 710055,
China. c
Life and Environment Science College, Shanghai Normal University, Shanghai 200234, China.
d
Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800, China
† These authors contributed equally to this work.
ABSTRACT: The existence of bulk nanobubbles are still controversial even though their significance in a large range of applications. Here, we developed a new method of compression-decompression to produce controllably bulk nanobubbles. Then we further investigated the generation of bulk nanobubbles in pure water, acid, alkaline and salt solutions using nanoparticle tracking analysis, respectively. The results indicated that the concentration of bulk nanobubbles depends on the decompression time and would reach to a maximum value when the decompression time is about 30 min for the pure water system. More importantly, we gave a relatively direct evidence of the existence of bulk nanobubbles by measuring the X-ray fluorescence intensity of Kr in acid, alkaline and salt solutions. It is shown that the decrease tendency in intensity of Kr in alkaline solution is similar to that in the concentration of bulk nanobubbles with the deposited time, indicating that the bulk nanobubbles produced are indeed gas inside. Furthermore, the concentration and stability of bulk nanobubbles in the alkaline solution are both greatest comparing with other two solutions regardless of gas types. The concentration of bulk nanobubbles will decrease in an order: alkaline > acid/pure water > salt solutions. We believe that our results should be very helpful for understanding the formation and stability of bulk nanobubbles in different solutions.
INTRODUCTION Nanoscale gas bubbles are significant to many industry-related research fields, such as nanoscopic cleaning,
1-3
controlling slip in microfluidics,
4-6
mineral flotation,
7-13
wastewater treatment,
8-9, 14-15
biomedical and chemical industries, etc..16-18 Different kinds of nanobubbles in the aforementioned applications usually exhibit distinguished physical and chemical properties because their activities are highly correlated with their unique condition,
6, 19-20
lifespan,
21-23
size
24-25
and stability.
26-29
It is well
known that nanoscale gas bubbles mainly include surface nanobubbles and bulk nanobubbles. Surface nanobubbles
31-35
6, 28, 30
are nanoscale gaseous domains aggregated on the hydrophobic/hydrophilic
substrates, and can survive for several days. Their existence was first predicted by Parker et al.
36
and
imaged directly in 2000 by Lou et al and Ishida et al using tapping mode atomic force microscopy. 37-38 However, for bulk nanobubbles their existence still remains controversial because of the lack of direct and sensitive detecting techniques.
30, 39
There is much skepticism associated with the existence and
stability of bulk nanobubbles. However, bulk nanobubbles are thought more significant than surface nanobubbles comparing with their application aspects to some extent even though their mechanism behind those applications is unknown. In the last decade, many techniques for bulk nanobubble
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fabrications have been reported. They included ultrasound, exchange,
45-46
and liquid cavitation,
11, 47
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40-42
introduction of gas,
etc. Also, Kukizaki et al
48
30, 43-44
solvent
presented the production of
uniformly sized nanobubbles using gas Shirasu-porous-glass membranes as the liquid dispersion medium. Recently, the cavitation tube
49
was used to generate a high concentration of nanobubbles with a high
potential. Although there are a lot of efforts on the study of bulk nanobubbles, further evidence and investigation on their mechanism is still needed. Also, the influences of different solutions on the properties of bulk nanobubbles are very important for the applications. The methods to produce and measure the bulk nanobubbles still need to be explored. Recently, we used nanoparticle tracking analysis (NTA) to detect the size and concentration of bulk nanobubbles produced by exchanging of ethanol and water, as well as cold water and decompressing. 45, 50-52 It was proved as a powerful tool to give the size distribution and concentration of bulk nanobubbles compared with conventional dynamic light scattering.
53-56
Another
powerful technique is synchrotron based X-ray fluorescence absorption which can provide the chemical information in bulk solution. 57 In this study, we developed a new method, compression-decompression, to produce bulk nanobubbles in different solutions. The concentration, size and stability of bulk nanobubbles in the acid, alkane and salt solutions were measured by NTA. More importantly, we further proved the bulk nanobubbles are indeed gas inside by Kr X-ray fluorescence absorption. Results showed that the concentration and stability of bulk nanobubbles in the alkaline solution are both greatest in the three solutions. Finally, we gave a possible explanation and discussion about those results.
MATERIALS AND METHODS Materials. Ethanol (≥99.8%, GR) was purchased from Sinopharm Chemical Reagent Co. Ltd. Beakers and syringes were immersed in chromic acid for 12 hours to remove organics, cleaned by ultrasound and dried at the room temperature in the vacuum chamber. The purity of N2 and Kr is 99.94% and 99.99%, respectively. Hydrochloric acid, sodium chloride and sodium hydroxide with analytical grade were purchased by Sinopharm Chemical Reagents Co., Ltd. Pure water with conductivity of 18.2 MΩ·cm used in the experiments was provided by an ELGA classic water purification system. Production of bulk nanobubbles. Bulk nanobubbles were produced by pressurizing gas into the solution and then slowly depressurizing it, we called compression-decompression method. Main steps are followed. Firstly, the solution was degassed for about 3 hours in a vacuum chamber and then was placed in a pressurized chamber at 10 atm for 10 min, during which gas (N2 or Kr) was compressed to the solution. Then, the pressure was released slowly to normal atmosphere. This releasing time was called decompression time. Then the solution was very quickly to inject to the cell of NTA for measurement. When starting to measure, we defined this time as zero, and deposited different time to measure again. Thus, we obtained different concentration and size distributions of nanobubbles at different deposited time. The nanobubbles would be produced during the decompression considering the extra gas will be released and the solution would reach to gas supersaturated state. Hydrochloric acid solution with a pH of 4.5, sodium hydroxide solution with a pH of 9.5 and sodium chloride solution (10-4 mol/L) were prepared and used in the experiments.
The measurement of bulk nanobubbles using NTA. The concentration and size distribution of nanobubbles were acquired by NTA (NS 300, Malvern). Equipped with a 20-fold magnification microscope and a high-speed camera, NTA depends on a laser light source (65mW, which is equal to 405 nm) to measure the size distribution and concentration of “nanoparticles”. When the laser impinges
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on the particle, it emerges a scattering spot. High-speed camera records the path of scattered light spots. Each result came from the average of five measurements, and the film lasted 60 seconds, capturing 20 frames per second. The camera level is usually set to 14, the threshold is set to 15, and the solution viscosity is 1CP. The optical field is fixed (about 80um) and the depth of the light beam is about 10 μm. The particle concentration can be obtained by dividing the volume of the field by the number of nanoparticles. The camera subsequently captures a video file of particles moving under Brownian motion within a field of view of approximately 100 μm × 80 μm × 10 μm. The size of nanoparticles is determined using the Stokes-Einstein equation: 𝐷𝑡 =
𝑇𝐾𝐵 3𝜋𝜂𝑑
where KB, T, and η are Boltzmann’s constant, the temperature, and the liquid viscosity, respectively, and Dt is the diffusion coefficient, which is an experimentally measured value based on the Brownian motion of the particle.
The micro X-ray fluorescence spectra experiments. The hard X-ray absorption intensity of Kr in different solutions prepared in 2.2 parts was obtained at the beamline 15 U in Shanghai Synchrotron Radiation Facility (SSRF). The photon energy was set to be 14.5 keV for Kr (KL3) measurements. A focused beam with spot size of about 2.2 μm × 2.5 μm was used. Step size was set as 2.0 μm and the collecting time for each step was 20 ms. The experiments were repeated three times for each sample. Kr is chosen as a typical sample to prove that the solution contains a large concentration Kr. Those nanobubbles might be composed of gas Kr. By comparing X-ray fluorescence results and NTA data, we would provide the evidence that “nanoparticles” measured by NTA are Kr contained nanobubbles.
RESULTS AND DISCUSSION The generation of bulk nanobubbles in pure water by compression-decompression method. First, we developed a new method, compression-decompression method, to produce bulk nanobubbles. The nitrogen and pure water were used in this experiment. The produced process was described as experimental part. NTA was used to measure the concentration of formed bulk nanobubbles. Figure 1 presented that the concentration of produced bulk nanobubbles as a function of decompression and deposited time. As shown in Figure 1a, the concentration of bulk nanobubbles in pure water increases with the decompression time increases. When the decompression time reaches 30 min, the concentration of bulk nanobubbles is maximum (approximately 5.8×107 particles/mL). With the decompression time further increases, the concentration of bulk nanobubbles slightly decreased. So, the decompression time was set at 30 min in the subsequent experiments. Using the compression-decompression method, we can produce a large amount of bulk nanobubbles, approximately 5.8×107 particles/mL in pure water. Next, we studied the stability of bulk nanobubbles formed after the 30min decompression time in pure water. As showed in Figure 1b, the concentration of bulk nanobubbles slowly increases while the deposited time is from 0 to 2 h. The emergence of this phenomenon may be related to the solubility 58 and evolution rate of the gas. 59-60 And then at 2.5 h, the concentration of nanobubbles increased sharply, which may be because the degree of gas supersaturation in the solution reached the maximum at this time. Among 2.5 h and 4.5 h, a stable platform appeared, and the concentration of bulk nanobubbles kept at about 108 particles/mL, then it reached a maximum peak at 3.5 h, about 1.31×108 particles/mL. The longevity of up to 5 h may very useful for the application of bulk nanobubbles.
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Figure 1. (a) The concentration of bulk nanobubbles in pure water after compressing for 10 min at 10 atm with different decompression time for 0 min, 10 min, 20 min, 30 min and 40 min, respectively. (b) The concentration of bulk nanobubbles after 30min decompression as a function of deposited time.
The generation and stability of bulk nanobubbles in hydrochloric acid solution. Above results showed that the method of compression-decompression is an easy way to produce a large number of bulk nanobubbles. Next, we would like to compare the formation and stability of bulk nanobubbles in acid, alkali and salt solutions. First, we measured the concentration of bulk nanobubbles produced by compression-decompression in hydrochloric acid solution with a pH of 4.5. The control experiment was also performed without performing the process of compression and decompression and just acid solution as prepared. The main results are shown in Figure 2. In Figure 2a, it can be seen that the nanobubbles in hydrochloric acid solution without compression-decompression are not stable with the deposited time. The possible reason is that H+ ions were adsorbed on the surface of nanobubbles to cause the negative surface potential, 61-62 resulting in the decrease of electrostatic repulsive force among nanobubbles. After compression-decompression, the concentration of formed bulk nanobubbles is larger and more stable relatively than those without disposed. The average sizes of bulk nanobubbles formed with the deposited time were showed in Figure 2b. The results showed that the average size of bulk nanobubbles through decompression is smaller than that in the original solution, which may be related to the gas evolution rate.
Figure 2. The concentration (a) and average size (b) of nanobubbles in hydrochloric acid solution with and without decompression (control) as a function of deposited time.
The generation and stability of bulk nanobubbles in sodium hydroxide solution. The concentration and size of bulk nanobubbles were obtained by NTA in the sodium hydroxide solution
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with a pH of 9.5 with and without compression-decompression. The typical results were shown in Figure 3. In Figure 3a, it can be seen that the concentration of nanobubbles produced by compressiondecompression in sodium hydroxide solution reaches at an optimal value (3.25×108 particles/ml) at the beginning. Despite there is a decreasing trend, the concentration of bulk nanobubbles in the solution is very larger than the control system without disposing. After 5 h, the concentration of bulk nanobubbles in the solution still remains 1.0×108 particles/ml. Figure 3b showed the average size of the nanobubbles produced by compression-decompression is mainly distributed in the range of 150 to 200 nm. In contrast, the average size of nanobubbles fluctuates greatly in the control system. This phenomenon might be explained that hydroxyl ions contained in the alkaline solution are also negative and same as negatively charged
62
with the nanobubbles
63-64
and the stable repulsive force between the two charges makes it
possible that the nanobubbles become more stable. From the electrostatic repulsion, the isoelectric point of the nanobubble surface is at a pH range of 3-4, the zeta potential of the nanobubble surface is negative under alkaline conditions, causing a large electrostatic repulsion between bubbles and bubbles, and thus the bubbles are relatively stable under alkaline conditions. Therefore, it can be inferred that the external negative electrostatic pressure generated by the charged nanobubble interface under alkaline conditions balances the Laplace pressure
65
inside the nanobubbles, so that the gas does not diffuse during the
equilibrium, and thus the nanobubbles are more stable.
Figure 3. The concentration (a) and average size (b) of bulk nanobubbles in the sodium hydroxide solution with and without compression-decompression as a function of deposited time.
The generation and stability of bulk nanobubbles in sodium chloride solution. The concentration and average size of bulk nanobubbles in sodium chloride solution with a concentration of 1.0×10-4 mol/L with and without compression-decompression as a function of deposited time are shown in Figure 4. In Figure 4a, it can be apparently seen that the concentration of bulk nanobubbles formed after compression-decompression in sodium chloride solution is not very high. The highest value is only 3.0×107 particles/ml, just a little more than that of bulk nanobubbles in the previous pure water. But this value is still larger than the control system. In Figure 4b, we can find that the average size of nanobubbles in gassed solution slightly increased from 175 to 300 nm before 4.5h. The concentration of bulk nanobubbles in the salt solution in control is relatively low to the previous alkaline solutions.
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Figure 4. The concentration (a) and average size (b) of bulk nanobubbles in sodium chloride solution with and without compression-decompression as a function of deposited time.
The possible evidence of bulk nanobubbles. It may still ask a question whether the bulk nanobubbles formed above are real gas inside or not even though we presented their formation depends on the decompressing time. Therefore, we measured the X-ray fluorescence absorption near Kr L edge to confirm the system contains a large number of Kr. At the same time, the NTA experiments also were performed with the same samples. We chose firstly sodium hydroxide solution as a typical system based on above results which showed that a large number of bulk nanobubbles could be produced comparing other systems. The sample was measured quickly after decompressing 30 min while injecting Kr at 10 atm for 10min. Figure 5a gave the dependence of concentration of bulk nanobubbles in sodium hydroxide solution on deposited time. It was found that the concentration is gradually reduced with the deposited time, which is consistent with the change of nitrogen system showed in Figure 3a. The same samples were measured by X-ray fluorescence at the same time. As shown in Figure 5b, the intensity of Kr absorption decreases with the deposited time. The tendency of decreasing is consistent with the decreased concentration of bulk nanobubbles measured by NTA in Figure 5a. It indicated that the content of bulk nanobubbles formed should be from Kr. Then we measured Kr -containing acid and salt solution. The main results were showed in Figure 5c. The intensity of Kr in sodium hydroxide solution is strongest among three systems, which also agrees with previous results that a largest amount of bulk nanobubbles could be produced in sodium hydroxide solution comparing with acid and salt solutions at the same condition. It also further proves the formed bulk nanobubbles are related with the amount of Kr.
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Figure 5. (a) The concentration of bulk nanobubbles in the Kr containing sodium hydroxide solution as a function of the deposited time. (b) The variation of Kr absorbed intensity with the deposited time. (c)The variation of Kr absorbed intensity in the acid, alkaline and salt solutions with the deposited time, respectively.
Based on above results, we would like to compare the formation and stability of bulk nanobubbles in pure water, acid, alkaline and salt solutions. Firstly, we developed a new method to produce bulk nanobubbles by measuring the pure water system. It was found that the formation of bulk nanobubbles depends on the decompression time. The fast releasing of gassing may cause the release of gas from the solution and less nanoscale gas bubbles formation. Then we studied the formation and stability of bulk nanobubbles in acid, alkaline and salt solutions. More interestingly, we found that the concentration of bulk nanobubbles in alkaline are higher than in other solutions. We summarized the data in Figure 6a. The ability of stabilized bulk nanobubbles has the order: alkaline > acid/pure water > salt solution. Here, we cannot give a confirmed reason, but it should be relative to the charges in the solution. Negative charges are very helpful for the formation and stability of bulk nanobubbles as showed in Figure 6b. Another important result is that the concentration of bulk nanobubbles with different gases (N2 or Kr) seems similar level as showed in Figure 5c comparing with the data in Figure 2a, 3a and 4a. It should be noted that it needs to study more gas to further confirm in the future.
Figure 6. (a) The concentration comparison of bulk nanobubbles in hydrochloric acid solution, sodium hydroxide solution and sodium chloride solution after compression-decompression. (b) The probable mechanism of hydroxyl ion and bulk nanobubbles in solutions.
CONCLUSIONS In summary, we reported that a new method of compression-decompression could be used to generate a larger number of bulk nanobubbles. The concentration and average size of bulk nanobubbles formed as well as their stability with the deposited time were measured by NTA. The decompression time can affect
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the concentration of nanobubbles. We compared the formation and stability of bulk nanobubbles in pure water, acid, alkaline and salt solutions. More interestingly, the concentration of bulk nanobubbles in alkaline is much higher than in other solutions. We further gave the evidence of bulk nanobubbles by measuring the X-ray fluorescence intensity of Kr that formed bulk nanobubbles should be Kr inside. Those results would be very useful for understanding the formation and stability of bulk nanobubbles in different solutions and their potential applications.
AUTHOR INFORMATION
Corresponding Authors *E-mail
[email protected] (Y.D.). *E-mail
[email protected] (J.H.). *E-mail
[email protected] (L.Z.).
Notes The authors declare no competing financial interest.
ACKNOWLEDGMENTS
This work was supported by the National Natural Science Foundation of China (Nos. 11874379, 11575281, U1532260), and the Knowledge Innovation Program of the Chinese Academy of Sciences (No. QYZDJ-SSW-SLH019). The authors also thank the beamline 08U1A staffs at the Shanghai Synchrotron Radiation Facilities (SSRF) for their suggestions and helps.
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