Effects of Sample Preparation on Particle Size Distributions of Different Types of Silica in Suspensions
"> Figure 1
<p>SEM and TEM images of different silica types. (<b>a</b>) fumed (pyrogenic) silica (opened fractal-like aggregates), (<b>b</b>) precipitated silica (compact fractal-like aggregates), (<b>c</b>) silica gel (compact and microporous fractal-like aggregates) and (<b>d</b>) colloidal silica (isolated spherical nanoparticles or small aggregates, here dried on TEM grid to opened agglomerates).</p> "> Figure 2
<p>Progressive heating of the sonotrode, sample fluid, and beaker in the course of USD. Images were captured with a thermal imaging camera (Seek Thermal) after different dispersing periods; (<b>a</b>,<b>b</b>): 0 s, (<b>c</b>): 30 s, (<b>d</b>): 60 s. Temperature (in degree Celsius) is shown on a pseudo-color scale whose range was automatically adjusted to the temperature peak (T<sub>min</sub>/T<sub>max</sub>) of the measurement (i.e., (<b>a</b>) 17 °C/22 °C, (<b>b</b>) 17 °C/23 °C, (<b>c</b>) 17 °C/26 °C).</p> "> Figure 3
<p>Calorimetric calibration curves of ultrasonic dispersing instruments. (<b>a</b>) temperature increases (Δ<span class="html-italic">T</span>) in Kelvin (K) over time, obtained with a 13 mm tip diameter sonotrode (Branson 450D) and increasing amplitudes (10–60% from maximum, as indicated in the graph). (<b>b</b>) Heat production (<span class="html-italic">P</span><sub>cal</sub>, W) of the different dispersing instruments and sonotrode geometries Vibra-Cell 72412 (V), Topas UDS751 (T) and Branson SONIFIER 450F (B) (outlined in <a href="#nanomaterials-08-00454-t003" class="html-table">Table 3</a>) as a function of increasing amplitude (in % from maximum).</p> "> Figure 4
<p>Particle size distribution of PS (440 m<sup>2</sup>/g) dispersed by different procedures. (<b>a</b>) Size distribution measured by laser diffraction spectroscopy plotted as the transformed distribution density (q<sup>3</sup>*). Weak (PS), moderate (RS) and intense (US) dispersion with increasing ultrasonic energies (indicated in the diagram) were employed. (<b>b</b>) Silica suspensions after five months (left 1 J/mL, middle 270 J/mL, and right 1440 J/mL).</p> "> Figure 5
<p>Particle size distribution of FS (300 m<sup>2</sup>/g) dispersed by different procedures. (<b>a</b>) Size distribution measured by laser diffraction spectroscopy plotted as the transformed distribution density (q<sup>3</sup>*). Weak (PS), moderate (RS) and intense (US) dispersion with increasing ultrasonic energies (indicated in the diagram) were employed. (<b>b</b>) Silica suspensions after five months (left 1 J/mL, middle 270 J/mL, and right 1440 J/mL).</p> "> Figure 6
<p>Particle size distribution of SG (BET: 700 m<sup>2</sup>/g) dispersed by different procedures. (<b>a</b>) Size distribution measured by laser diffraction spectroscopy plotted as the transformed distribution density (q<sup>3</sup>*). Weak (PS), moderate (RS) and intense (US) dispersion with increasing ultrasonic energies (indicated in the diagram) were employed. (<b>b</b>) Silica suspensions after five months (left 1 J/mL, middle 270 J/mL, and right 1440 J/mL).</p> "> Figure 7
<p>Particle size distribution of silica suspension after administration of increasing dispersion energy as measured by laser diffraction. Curves show the trends for the x<sub>50,3</sub> and x<sub>99,3</sub> quantiles of the volume weighted size distribution. USD energy density of ultrasonic treatment is indicated in J/mL.</p> "> Figure 8
<p>Intensely dispersed SAS samples (USD, <span class="html-italic">E<sub>V</sub></span><sub>,cal</sub>: 1440 J/mL) after long-term sedimentation (5 months): (<b>a</b>) PS; (<b>b</b>) FS; (<b>c</b>) SG.</p> "> Figure 9
<p>Particle size distribution (PSD) of amorphous silica suspensions dispersed by two different ultrasonic dispersion energy densities (270 and 1440 J/mL). PSD was measured by dynamic light scattering (DLS). FS: fumed silica, SG: gel silica, PS: precipitated silica. (<b>a</b>) Intensity-weighted sum functions for different energy density values. (<b>b</b>) Intensity-weighted transformed distribution density functions for different energy density values. Logarithmic normal distribution.</p> "> Figure 10
<p>Particle size distribution of colloidal silica dispersed by different procedures measured by DLS. (<b>a</b>) Mean particle size (xcum) and corresponding polydispersity index (PDI) as determined with cumulant analysis. (<b>b</b>) Bottom view of a vial with an intensely dispersed colloidal silica sample (<span class="html-italic">E<sub>V</sub></span><sub>,cal</sub>: 1440 J/mL) taken after 5 months of gravitational settling.</p> "> Figure 11
<p>Comparison of new and used sonotrode with sonotrode abrasion as a consequence of long ultrasonic dispersion time (<b>a</b>,<b>b</b>); sonotrode abrasion sediment on the bottom of a precipitated silica suspension sample after high USD energy (<b>c</b>) (i.e., <span class="html-italic">E<sub>V</sub></span><sub>,cal</sub>: 1440 J/mL).</p> "> Figure 12
<p>Scanning electron microscope image of wear particles from the sonotrode tip. Abrasion particles were collected from the sediment of a silica suspension sample after high USD energy (i.e., <span class="html-italic">E<sub>V</sub></span><sub>,cal</sub>: 1440 J/mL).</p> "> Figure 13
<p>(<b>a</b>) Light microscope image of polymer gaze for size-selective suspension filtration and (<b>b</b>) <span class="html-italic">T</span>(<span class="html-italic">x</span>): grade efficiency function after gaze test filtration with glass spheres.</p> "> Figure 14
<p>(<b>a</b>) filter grade efficiency curve and calculated results for penetrated (filtrate) and retained particle size distributions from feed size distribution (yellow) in comparison to not filtered but with 1440 J/mL dispersed sample (<b>b</b>) Evolution of PSD during ultrasonication of precipitated silica (440 m<sup>2</sup>/g); cumulative distribution functions measured by LD.</p> ">
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Instruments and Procedures for Sample Preparation
2.3. Instruments for Particle Size Analysis
2.4. Estimation of the Calorimetric Energy Input
3. Results and Discussion
3.1. Calorimetric Calibration of Probe Sonication
3.2. Sample Preparation by Probe Sonication
3.2.1. Impact of USD on Particle Size Distribution of SAS
3.2.2. Sample Contamination with Probe Sonication
3.3. Sample Preparation with Size-Selective Filtration
4. Conclusions
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Protocol | Sample Volume | Dispersing Time | (Calorimetric) Energy Density |
---|---|---|---|
Tantra 2016 [42]; Pradhan 2016 [43] | 6 mL | 16 min | 1176 J/mL |
Rasmussen et al., 2013 [35] | 15 mL 10 mL | 10 min 16 min | 500–400 J/mL 2500 J/mL |
Taurozzi et al., 2012 [44] | 50 mL | 5 min | 300 J/mL |
Jensen et al., 2011 [33] | 6 mL | 16 min | 3140 J/mL |
Bihari et al., 2008 [45] | 1 mL | 1 min | 420 J/mL |
Mandzy et al., 2005 [46] | - | Time frames (2 h) | 5700 J/mL |
Pohl et al., 2005 [37] | 10–42 mL | 17–630 s | 400–30,000 J/mL |
Pohl et al., 2004 [47] | 3–6 mL | - | 100–2000 J/mL |
SAS Type Internal Code | Fumed Silica F-3 | Precipitated Silica P-2 | Silica Gel G-1 | Colloidal Silica C-1 |
---|---|---|---|---|
BET 1 (m2/g) | 300 | 440 | 700 | 200 2 |
solid content for suspensions (wt.-%) | - | - | - | 40 |
pH 3 | 5 | 6.5 | 4.4 | 9.7 |
electric conductivity (μS/cm) at 25 °C | 4 | 160 | 55 | 4771.6 |
Model | Vibra-Cell 72412 1 | UDS751 2 | SONIFIER 450D 3 |
---|---|---|---|
Code | V | T | B |
company | Sonics and Materials | Topas GmbH | Branson Ultrasonics |
normal capacity (W) | 600 | 200 | 400 |
tip diameter (Ø, mm) | 13 19 | 3 7 14 | 5 13 |
amplitude (%) | 0–100 | 0–100 | 10–100 |
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Retamal Marín, R.R.; Babick, F.; Lindner, G.-G.; Wiemann, M.; Stintz, M. Effects of Sample Preparation on Particle Size Distributions of Different Types of Silica in Suspensions. Nanomaterials 2018, 8, 454. https://doi.org/10.3390/nano8070454
Retamal Marín RR, Babick F, Lindner G-G, Wiemann M, Stintz M. Effects of Sample Preparation on Particle Size Distributions of Different Types of Silica in Suspensions. Nanomaterials. 2018; 8(7):454. https://doi.org/10.3390/nano8070454
Chicago/Turabian StyleRetamal Marín, Rodrigo R., Frank Babick, Gottlieb-Georg Lindner, Martin Wiemann, and Michael Stintz. 2018. "Effects of Sample Preparation on Particle Size Distributions of Different Types of Silica in Suspensions" Nanomaterials 8, no. 7: 454. https://doi.org/10.3390/nano8070454