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Environmental chamber for in situ dynamic control of temperature and relative humidity during x-ray scattering
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10.1063/1.3685753
/content/aip/journal/rsi/83/2/10.1063/1.3685753
http://aip.metastore.ingenta.com/content/aip/journal/rsi/83/2/10.1063/1.3685753

Figures

Image of FIG. 1.
FIG. 1.

Specimen chamber 3D illustration. The specimen chamber includes the following components: (1) RH chamber, (2) sample mount, (3) door, (4) sample clamp, (5) window frames, (6) y-direction motor mount for vertical displacement, (7) insulator, (8) strain relief, (9) insulator for strain relief, (10) cooling loops, and (11) beryllium (Be) window. Key features of this new design include large escape angle (x-ray scattering angle 2θ = ±30°, horizontal), compatibility with an evacuated x-ray chamber, capability to hold multiple samples, dynamic control of temperature and relative humidity, and computer control of temperature and relative humidity integrated with data collection.

Image of FIG. 2.
FIG. 2.

Process control instrumentation flow diagram. Here, water recirculating bath temperature, bottle temperature, HT1 and HT2, and gas flow rates are the controlled variables. The system incorporates four continuous process controls and two manipulated variables. The control loop feedback mechanism regulates the saturation level of the gas by controlling the dry and saturated gas inlet flows using Eq. (1).

Image of FIG. 3.
FIG. 3.

Measured temperature (a) and relative humidity (b) for the EC when the temperature is set to 30 °C and the relative humidity is changes stepwise. The measured temperature is controlled to a precision of ± 0.05 °C. The standard deviation of the %RH is reported in part b and is 0.4–1.41% RH.

Image of FIG. 4.
FIG. 4.

Measured temperature (a) and relative humidity (b) for the EC when the temperature is set to 80 °C and the relative humidity is changes stepwise. The measured temperature is controlled to a precision of ± 0.38 °C. The standard deviation of the %RH is reported in part b and is 1.25–3.18% RH.

Image of FIG. 5.
FIG. 5.

X-ray scattering through the environmental chamber without a sample as a function of relative humidity at 60 °C. Attenuation due to Be windows, nitrogen and water molecules is minimal.

Image of FIG. 6.
FIG. 6.

Chemical structures for (a) Nafion® polymer and (b) poly(1-[(2-methacryloyloxy)ethyl]-3-butlyimidazolium-hydroxide) (poly(MEBIM-OH)).

Image of FIG. 7.
FIG. 7.

2D x-ray scattering pattern (at 86% RH, 25 °C) of (a) Nafion® cast film and (b) Nafion® nanofiber (arrow indicating longitude direction of fibers).20 X-ray scattering profile as a function of relative humidity for (c) Nafion® cast film and (d) Nafion® nanofibers. The x-ray scattering data are shifted vertically for clarity.

Image of FIG. 8.
FIG. 8.

X-ray scattering profile as a function of relative humidity for a polymerized ionic liquid. The x-ray scattering profiles are shifted vertically for clarity.

Tables

Generic image for table
Table I.

Environmental chamber (EC) descriptions and capabilities.

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/content/aip/journal/rsi/83/2/10.1063/1.3685753
2012-02-21
2014-04-20
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752b84549af89a08dbdd7fdb8b9568b5 journal.articlezxybnytfddd
Scitation: Environmental chamber for in situ dynamic control of temperature and relative humidity during x-ray scattering
http://aip.metastore.ingenta.com/content/aip/journal/rsi/83/2/10.1063/1.3685753
10.1063/1.3685753
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