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In situ multipurpose time-resolved spectrometer for monitoring nanoparticle generation in a high-pressure fluid
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10.1063/1.4737886
/content/aip/journal/rsi/83/7/10.1063/1.4737886
http://aip.metastore.ingenta.com/content/aip/journal/rsi/83/7/10.1063/1.4737886

Figures

Image of FIG. 1.
FIG. 1.

(a) Side-view and top-view cross sections of high-pressure optical cell. (b) Photograph of high-pressure optical cell: (i) cartridge heaters, (ii) fluid inlet–outlet ports, (iii) thermocouple, (iv) magnetic stirrer. (c) Schematic of clamped-type and unclamped-type flanges for holding window. The labels p and D represent the pressure load on the window and the diameter of effective supporting area, respectively.

Image of FIG. 2.
FIG. 2.

Schematic of system for controlling pressure and temperature of optical cell. V1 is a diaphragm sealed valve as a feed valve; V2 is a diaphragm sealed valve as a stop valve; F is a membrane filter with a pore size of 0.1 μm for increasing the optical purity of the fluid; T is a pressure transducer used for pressures ≤30 MPa; IA is an instrumentation amplifier of pressure transducer; R is a pressure regulator, secondary venting pressure ≤0.3 MPa; VT is a voltage transformer; SSR is a solid-state relay used for currents ≤10 A; PID is a PID controller.

Image of FIG. 3.
FIG. 3.

Schematic of optical configurations of the three spectrometers. (a) Transient absorption spectrometer, (b) absorption spectrometer for long delay times, and (c) DLS spectrometer. Nd:YAG laser generates the pump light for conducting PLA for the three spectrometers; WP is a half-wave plate; Ms are reflecting mirrors, FMs are flipping mirrors; Ss are shutters; CL is a cylindrical lens; Ls are lenses; OFs are optical fibers; PHs are pinholes; and lamps include a halogen and D2 lamp.

Image of FIG. 4.
FIG. 4.

In situ transient absorption spectra of gold nanoparticles in supercritical CO2 measured by developed system. The spectra are collected and the gold nanoparticles are generated by PLA in supercritical CO2 at reduced densities ρ r = ρ/ρ c = 0.2 and 0.8 and at reduced temperature T r = T/T c = 1.04, where ρ c and T c are the critical density and temperature, respectively.

Image of FIG. 5.
FIG. 5.

Time evolutions of in situ absorption spectra of gold nanoparticles measured by developed absorption spectrometer. The spectra are collected in situ and the gold nanoparticles are generated by PLA in supercritical CO2 at reduced densities ρ r = ρ/ρ c = 0.2, 0.6, 1.0, and 1.4 and at a reduced temperature T r = T/T c = 1.02, where ρ c and T c are the critical density and temperature, respectively.

Image of FIG. 6.
FIG. 6.

In situ time correlation functions of gold nanoparticles measured by developed DLS instrument. The correlation functions are collected in situ and the gold nanoparticles are generated by PLA in supercritical CHF3 at reduced densities ρ r = ρ/ρ c = 0.2, 0.4, and 0.7 and at a reduced temperature T r = T/T c = 1.02, where ρ c and T c are the critical density and temperature, respectively.

Image of FIG. 7.
FIG. 7.

In situ size distribution functions of gold nanoparticles obtained from the analysis of time correlation functions of Figure 6. The size distribution functions were collected in situ and the gold nanoparticles are generated by PLA in supercritical CHF3 at reduced densities ρ r = ρ/ρ c = 0.2, 0.4, and 0.7 and at a reduced temperature T r = T/T c = 1.02, where ρc and T c are the critical density and temperature, respectively.

Tables

Generic image for table
Table I.

Critical constants of typically used fluids.

Generic image for table
Table II.

Calculated stress areas and engaged lengths for ISO metric screws.

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/content/aip/journal/rsi/83/7/10.1063/1.4737886
2012-07-26
2014-04-25
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752b84549af89a08dbdd7fdb8b9568b5 journal.articlezxybnytfddd
Scitation: In situ multipurpose time-resolved spectrometer for monitoring nanoparticle generation in a high-pressure fluid
http://aip.metastore.ingenta.com/content/aip/journal/rsi/83/7/10.1063/1.4737886
10.1063/1.4737886
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