Application of Grazing Incidence X-Ray Diffraction to Polymer Blends

1992 ◽  
Vol 36 ◽  
pp. 373-377
Author(s):  
Mary F. Garbauskas ◽  
Donald G. LeGrand ◽  
Raymond P. Goehner

AbstractThe physical properties of polymer blends consisting of one or more crystallizable components are affected by the microstructure of these materials. In particular, the degree of crystallinity can be influenced by processing parameters, and the crystallinity, as well as the phase distribution, may vary as a function of depth through an injection molded part. Conventional x-ray diffraction techniques can provide information regarding both phase composition and degree of crystallinity, but, because of the relative transparency of these materials to wavelengths generally available in the laboratory, these techniques provide information representative of only the bulk. By employing parallel beam optics at varying grazing incidence angles, the x-ray sampling depth can be varied without loss of resolution, This technique can be used to vary the effective analysis depth from the top several hundred angstroms for low grazing incidence to centimeters for transmission diffraction patterns, Grazing incidence techniques have found initial application in the characterization of thin metallic and ceramic films. This paper demonstrates the feasibility of using parallel beam optics to depth profile low atomic number materials. The specific application of this technique to the characterization of injection molded polymers, including a blend of bisphenol-A polycarbonate (PC) and polybutylene terephthalate (PBT), will be presented.

2020 ◽  
Vol 35 (S1) ◽  
pp. S29-S33
Author(s):  
Dieter Ingerle ◽  
Werner Artner ◽  
Klaudia Hradil ◽  
Christina Streli

A commercial Empyrean X-ray diffractometer was adapted for combined grazing incidence X-ray fluorescence analysis (GIXRF) measurements with X-ray reflectivity (XRR) measurements. An energy-dispersive silicon drift detector was mounted and integrated in the angle-dependent data acquisition of the Empyrean. Different monochromator/X-ray optics units have been compared with the values obtained by the Atominstitut GIXRF + XRR spectrometer. Data evaluation was performed by JGIXA, a special software for combined GIXRF + XRR data fitting, developed at Atominstitut. A sample consisting of a ~50 nm nickel layer on a silicon substrate was used to compare the performance criteria (i.e. divergence and intensity) of the incident beam optics. An Empyrean X-ray diffractometer was successfully refitted to measure both GIXRF and XRR data.


1988 ◽  
Vol 32 ◽  
pp. 311-321 ◽  
Author(s):  
R.A. Larsen ◽  
T.F. McNulty ◽  
R.P. Goehner ◽  
K.R. Crystal

AbstractThe use of conventional θ/2θ diffraction methods for the characterization of polycrystalline thin films is not in general a satisfactory technique due to the relatively deep penetration of x-ray photons in most materials. Glancing incidence diffraction (GID) can compensate for the penetration problems inherent in the θ/2θ geometry. Parallel beam geometry has been developed in conjunction with GID to eliminate the focusing aberrations encountered when performing these types of measurements. During the past yearwe developed a parallel beam attachment which we have successfully configured to a number of systems.


2000 ◽  
Vol 07 (04) ◽  
pp. 437-446 ◽  
Author(s):  
G. RENAUD

The application of X-rays to the structural characterization of surfaces and interfaces, in situ and in UHV, is discussed on selected examples. Grazing incidence X-ray diffraction is not only a very powerful technique for quantitatively investigating the atomic structure of surfaces and interfaces, but is also very useful for providing information on the interfacial registry for coherent interfaces or on the strain deformation, island and grain sizes for incoherent epilayers.


1976 ◽  
Vol 20 ◽  
pp. 393-402 ◽  
Author(s):  
Richard M. Chrenko

X-ray residual stress measurements have been made with a commercial portable X-ray diffraction apparatus that uses parallel beam optics and that was specifically designed for residual stress measurements. This machine differs from X-ray diffraction units using the usual parafocusing geometry in several respects, most notably reduced sample placement errors and larger sample sizes that can be accommodated. Two special modes of operation are available and will be discussed. These are the ability to use the side inclining method for stress analysis and the ability to use an oscillating ψ motion, the latter mode being useful for examining large grain size materials.


1998 ◽  
Vol 13 (9) ◽  
pp. 2580-2587 ◽  
Author(s):  
K. H. Ryu ◽  
J-M. Yang

The characteristics of nanosized silicon nitride powders with doped Y2O3 and Al2O3 fabricated by a plasma-reacted chemical process were investigated. The chemical compositions of the powders were analyzed by wet chemical analysis. The morphology and the size distribution were determined by transmission electron microscopy (TEM). TEM with energy dispersive spectroscopy (EDS) was used to verify the existence of sintering additives in each individual particle. The crystal structure of the powders was identified by the selected area diffraction pattern (SADP). X-ray diffraction (XRD) technique was used for phase analysis and the measurement of degree of crystallinity. The characteristics of chemical bonding was analyzed by using Fourier transform infrared spectroscopy (FTIR).


2012 ◽  
Vol 528 ◽  
pp. 35-38 ◽  
Author(s):  
Ping Qu ◽  
Xuan Wang ◽  
Li Ping Zhang

Reinforcement of polymer with plant whiskers is a way of improving mechanical properties. Cellulose nanowhiskers (CNW) were separated from commercially available wood pulpboard. Different microscopy techniques, thermal gravimetric analysis, X-ray diffraction were used to study the structure and properties of the microcrystalline cellulose (MCC) and CNW. Because of the high specific surface area of CNW, the increases in total amorphous character of the cellulose decrease the relative degree of crystallinity. After chemical and physical treatment, the CNW in the length of several μm and diameters ranging from 20 - 50 nm was obtained. Both the initial decomposing temperature and temperature of maximum decomposing rate of CNW is higher than MCC, but lower than wood pulpboard.


2013 ◽  
Vol 2013 ◽  
pp. 1-4 ◽  
Author(s):  
Dandan Sun ◽  
Jiang Li ◽  
Qinghua Pan ◽  
Chaowei Hao ◽  
Guoqiao Lai

PA6/LiCl composites were synthesized by in situ anionic polymerization based on the interaction between the inorganic salts and PA6. Sodium hydroxide as initiator and N-acetylcaprolactam as activator were used in the preparation of PA6/LiCl composites with variety of LiCl content. X-ray diffraction (XRD) and differential scanning calorimeter (DSC) testing results showed that both of degree of crystallinity and melting temperature of the composites were decreased under the influence of LiCl. And theγcrystal phase proportion increased with increasing the LiCl content to appropriate amount.


Author(s):  
Naoshi Kawamoto ◽  
Hideharu Mori ◽  
Koh-hei Nitta ◽  
Shintaro Sasaki ◽  
Nobuhiko Yui ◽  
...  

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