In situ coupling of atomic force microscopy and sub-micrometer focused X-ray techniques

2014 ◽  
Vol 1712 ◽  
Author(s):  
Thomas W. Cornelius ◽  
Zhe Ren ◽  
Francesca Mastropietro ◽  
Simon Langlais ◽  
Anton Davydok ◽  
...  
Keyword(s):  
Mechanical Response ◽  
Elemental Distribution ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cu Nanowires ◽  
Force Microscopy ◽  
Indentation Tests ◽  
Scanning Force ◽  
Diffraction Patterns

ABSTRACTA scanning force microscope for in situ nanofocused X-ray studies (SFINX) has been developed which can be installed on diffractometers at synchrotron beamlines allowing for the combination with various techniques such as coherent X-ray diffraction and fluorescence. The capabilities of this device are demonstrated on Cu nanowires and on Au islands grown on sapphire (0001). The sample topography, crystallinity, and elemental distribution of the same area are investigated by recording simultaneously an AFM image, a scanning X-ray diffraction map, and a fluorescence map. Additionally, the mechanical response of Au islands is studied by in situ indentation tests employing the AFM-tip and recording 2D X-ray diffraction patterns during mechanical loading.

Growth and Characterization of bulk GaN by Ga Vapor Transport

2004 ◽  
Vol 831 ◽  
Author(s):  
Phanikumar Konkapaka ◽  
Huaqiang Wu ◽  
Yuri Makarov ◽  
Michael G. Spencer
Keyword(s):  
Growth Rates ◽  
Vapor Transport ◽  
Spiral Growth ◽  
X Ray Diffraction ◽  
X Ray ◽  
Force Microscopy ◽  
Atomic Force ◽  
Bulk Gan ◽  
Diffraction Patterns

ABSTRACTBulk GaN crystals of dimensions 8.5 mm × 8.5 mm were grown at growth rates greater than 200μm/hr using Gallium Vapor Transport technique. GaN powder and Ammonia were used as the precursors for growing bulk GaN. Nitrogen is used as the carrier gas to transport the Ga vapor that was obtained from the decomposition of GaN powder. During the process, the source GaN powder was kept at 1155°C and the seed at 1180°C. Using this process, it was possible to achieve growth rates of above 200 microns/hr. The GaN layers thus obtained were characterized using X-Ray diffraction [XRD], scanning electron microscopy [SEM], and atomic force microscopy [AFM]. X-ray diffraction patterns showed that the grown GaN layers are single crystals oriented along c direction. AFM studies indicated that the dominant growth mode was dislocation mediated spiral growth. Electrical and Optical characterization were also performed on these samples. Hall mobility measurements indicated a mobility of 550 cm2/V.s and a carrier concentration of 6.67 × 1018/cm3

Large Area Supersonic Jet Epitaxy of AlN, GaN, and SiC on Silicon

1996 ◽  
Vol 449 ◽  
Author(s):  
L.J. Lauhon ◽  
S. A. Ustin ◽  
W. Ho
Keyword(s):  
Supersonic Jet ◽  
X Ray Diffraction ◽  
Large Area ◽  
Free Jets ◽  
X Ray ◽  
Force Microscopy ◽  
Atomic Force ◽  
Supersonic Jet Epitaxy ◽  
Carrier Gases

ABSTRACTAlN, GaN, and SiC thin films were grown on 100 mm diameter Si(111) and Si(100) substrates using Supersonic Jet Epitaxy (SJE). Precursor gases were seeded in lighter mass carrier gases and free jets were formed using novel slit-jet apertures. The jet design, combined with substrate rotation, allowed for a uniform flux distribution over a large area of a 100 mm wafer at growth pressures of 1–20 mTorr. Triethylaluminum, triethylgailium, and ammonia were used for nitride growth, while disilane, acetylene, and methylsilane were used for SiC growth. The films were characterized by in situ optical reflectivity, x-ray diffraction (XRD), atomic force microscopy (AFM), and spectroscopic ellipsometry (SE).

(G03 Best Paper Award Winner) Analysis of Sn Behavior During Ni/GeSn Solid-State Reaction by Correlated X-ray Diffraction, Atomic Force Microscopy, and Ex-situ/In-situ Transmission Electron Microscopy

2020 ◽  
Vol MA2020-02 (24) ◽  
pp. 1750-1750
Author(s):  
Andrea Quintero Colmenares ◽  
Patrice Gergaud ◽  
Jean-Michel Hartmann ◽  
Vincent Delaye ◽  
Nicolas Bernier ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Ex Situ ◽  
Paper Award ◽  
X Ray Diffraction ◽  
Award Winner ◽  
X Ray ◽  
Force Microscopy ◽  
Atomic Force ◽  
Transmission Electron

Development of an in situ synchrotron X-ray total scattering setup under pressurized hydrogen gas

2018 ◽  
Vol 51 (3) ◽  
pp. 796-801 ◽  
Author(s):  
Kouji Sakaki ◽  
Hyunjeong Kim ◽  
Akihiko Machida ◽  
Tetsu Watanuki ◽  
Yoshinori Katayama ◽  
...  
Keyword(s):  
Pair Distribution Function ◽  
Hydrogen Gas ◽  
Ex Situ ◽  
Sample Holder ◽  
Hydrogen Storage Materials ◽  
X Ray Diffraction ◽  
Total Scattering ◽  
X Ray ◽  
Diffraction Patterns

This article describes the development of an in situ gas-loading sample holder for synchrotron X-ray total scattering experiments, particularly for hydrogen storage materials, designed to collect diffraction and pair distribution function (PDF) data under pressurized hydrogen gas. A polyimide capillary with a diameter and thickness of 1.4 and 0.06 mm, respectively, connected with commercially available Swagelok fittings was used as an in situ sample holder. Leakage tests confirmed that this sample holder allows 3 MPa of hydrogen gas pressure and 393 K to be achieved without leakage. Using the developed in situ sample holder, significant background and Bragg peaks from the sample holder were not observed in the X-ray diffraction patterns and their signal-to-noise ratios were sufficiently good. The PDF patterns showed sharp peaks in the r range up to 100 Å. The results of Rietveld and PDF refinements of Ni are consistent with those obtained using a polyimide capillary (1.0 mm diameter and 0.04 mm thickness) that has been used for ex situ experiments. In addition, in situ synchrotron X-ray total scattering experiments under pressurized hydrogen gas up to 1 MPa were successfully demonstrated for LaNi4.6Cu.

scholarly journals A Flow-Through Reaction Cell for Studying Minerals Leaching by In-Situ Synchrotron Powder X-ray Diffraction

Minerals ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 990
Author(s):  
Fatemeh Nikkhou ◽  
Fang Xia ◽  
Xizhi Yao ◽  
Idowu A. Adegoke ◽  
Qinfen Gu ◽  
...  
Keyword(s):  
Flow Rate ◽  
Pressure Leaching ◽  
X Ray Diffraction ◽  
Reaction Cell ◽  
Time Resolved ◽  
X Ray ◽  
Ore Minerals ◽  
Flow Through ◽  
Diffraction Patterns

A flow-through reaction cell has been developed for studying minerals leaching by in-situ time-resolved powder X-ray diffraction, allowing for a better understanding of the leaching mechanisms and kinetics. The cell has the capability of independent control of temperature (up to 95 °C) and flow rate (>0.5 mL min−1) for atmospheric pressure leaching. It was successfully tested at the powder diffraction beamline at the Australian Synchrotron. Galena powder was leached in a citrate solution under flow-through condition at a flow rate of 0.5 mL min−1, while diffraction patterns were collected during the entire leaching process, showing rapid galena dissolution without the formation of secondary mineral phases. The flow-through cell can be used to study leaching processes of other ore minerals.

scholarly journals In-situhigh-pressure powder X-ray diffraction study of α-zirconium phosphate

2014 ◽  
Vol 70 (3) ◽  
pp. 510-516
Author(s):  
Jennifer E. Readman ◽  
Alistair Lennie ◽  
Joseph A. Hriljac
Keyword(s):  
High Pressure ◽  
Synchrotron Radiation ◽  
Zirconium Phosphate ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
X Ray ◽  
Additional Water ◽  
Diffraction Patterns ◽  
Layered Phosphate

The high-pressure structural chemistry of α-zirconium phosphate, α-Zr(HPO4)2·H2O, was studied usingin-situhigh-pressure diffraction and synchrotron radiation. The layered phosphate was studied under both hydrostatic and non-hydrostatic conditions and Rietveld refinement carried out on the resulting diffraction patterns. It was found that under hydrostatic conditions no uptake of additional water molecules from the pressure-transmitting medium occurred, contrary to what had previously been observed with some zeolite materials and a layered titanium phosphate. Under hydrostatic conditions the sample remained crystalline up to 10 GPa, but under non-hydrostatic conditions the sample amorphized between 7.3 and 9.5 GPa. The calculated bulk modulus,K0= 15.2 GPa, showed the material to be very compressible with the weak linkages in the structure of the type Zr—O—P.

Statistical measures of spottiness in diffraction rings

2013 ◽  
Vol 47 (1) ◽  
pp. 166-172 ◽  
Author(s):  
Bridget Ingham
Keyword(s):  
Carbon Dioxide ◽  
Size Distribution ◽  
Intensity Variation ◽  
Incident Beam ◽  
Mean Square ◽  
X Ray Diffraction ◽  
X Ray ◽  
Statistical Measures ◽  
Diffraction Patterns

Spotty diffraction rings arise when the size distribution of crystallites illuminated by the incident beam includes crystallites that are large compared with the size of the beam. In this article, several statistical measures are used in conjunction to quantify spottiness and relate it to a crystallite size distribution: the number of peaks, the normalized root mean square intensity variation and the fractal dimension. These are demonstrated by way of example using synchrotron X-ray diffraction patterns collected duringin situcorrosion of mild steel in carbon dioxide-saturated aqueous brine.

In Situ X-Ray Diffraction Study of Thermal Stability of Cu and Cu-Zr Samples Processed by ECAP

2013 ◽  
Vol 753 ◽  
pp. 279-284 ◽  
Author(s):  
Radomír Kužel ◽  
Zdeněk Matěj ◽  
Miloš Janeček
Keyword(s):  
In Situ Measurements ◽  
X Ray Diffraction ◽  
X Ray ◽  
Abnormal Growth ◽  
Angular Pressing ◽  
Dislocation Densities ◽  
Diffraction Patterns ◽  
Number Of Passes ◽  
Thermal Stability Of

X-ray diffraction (XRD) studies of ECAP (equal-channel angular pressing) materials were performed after annealing and by in-situ measurements in XRD high-temperature chamber for samples prepared by different number of passes and number of revolutions, respectively. Main attention was given to Cu and Cu-Zr samples. Significant dependence on number of passes was found for ECAP samples. In-situ measurements were focused not only on temperature dependence but also on time evolution of the diffraction line profiles. Evaluation in terms of dislocation densities, correlation and crystallite size and its distribution was performed by our own software MSTRUCT developed for total powder diffraction pattern fitting. Abnormal growth of some grains with annealing is well-known for copper and leads to the creation of bimodal microstructure. Therefore a special care must be given to the evaluation and a model of two Cu components (larger and smaller crystallites) was fitted to the data if an indication of some crystallite growth appears either in the XRD line profile shape or in two-dimensional diffraction patterns.

In Situ X-ray Diffraction Study on the Orientation-Dependent Thermal Expansion of Cu Nanowires

2009 ◽  
Vol 113 (22) ◽  
pp. 9568-9572 ◽  
Author(s):  
Wen Fei Zhou ◽  
Guang Tao Fei ◽  
Xin Feng Li ◽  
Shao Hui Xu ◽  
Li Chen ◽  
...  
Keyword(s):  
Thermal Expansion ◽  
Diffraction Study ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cu Nanowires
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