Small-angle X-ray scattering

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Small-angle X-ray scattering (SAXS) is a small-angle scattering technique by which nanoscale density differences in a sample can be quantified. This means that it can determine nanoparticle size distributions, resolve the size and shape of (monodisperse) macromolecules, determine pore sizes, characteristic distances of partially ordered materials, and much more. [1] This is achieved by analyzing the elastic scattering behaviour of X-rays when travelling through the material, recording their scattering at small angles (typically 0.1 – 10°, hence the "Small-angle" in its name). It belongs to the family of small-angle scattering (SAS) techniques along with small-angle neutron scattering, and is typically done using hard X-rays with a wavelength of 0.07 – 0.2 nm. Depending on the angular range in which a clear scattering signal can be recorded, SAXS is capable of delivering structural information of dimensions between 1 and 100 nm, and of repeat distances in partially ordered systems of up to 150 nm. [2] USAXS (ultra-small angle X-ray scattering) can resolve even larger dimensions, [3] [4] [5] as the smaller the recorded angle, the larger the object dimensions that are probed.

Contents

SAXS and USAXS belong to a family of X-ray scattering techniques that are used in the characterization of materials. In the case of biological macromolecules such as proteins, the advantage of SAXS over crystallography is that a crystalline sample is not needed. Furthermore, the properties of SAXS allow investigation of conformational diversity in these molecules. [6] Nuclear magnetic resonance spectroscopy methods encounter problems with macromolecules of higher molecular mass (> 30–40 kDa). However, owing to the random orientation of dissolved or partially ordered molecules, the spatial averaging leads to a loss of information in SAXS compared to crystallography.

Applications

SAXS is used for the determination of the microscale or nanoscale structure of particle systems in terms of such parameters as averaged particle sizes, shapes, distribution, and surface-to-volume ratio. [7] [8] [9] [10] The materials can be solid or liquid and they can contain solid, liquid or gaseous domains (so-called particles) of the same or another material in any combination. Not only particles, but also the structure of ordered systems like lamellae, and fractal-like materials can be studied. The method is accurate, non-destructive and usually requires only a minimum of sample preparation. Applications are very broad and include colloids [11] , [12] , [13] , [14] of all types including interpolyelectrolyte complexes, [15] , [16] , [17] micelles, [18] , [19] , [20] , [21] , [22] microgels, [23] liposomes, [24] , [25] , [26] polymersomes, [27] , [28] metals, cement, oil, polymers, [29] , [30] , [31] , [32] plastics, proteins, [33] , [34] foods and pharmaceuticals and can be found in research as well as in quality control. The X-ray source can be a laboratory source or synchrotron light which provides a higher X-ray flux.

Resonant small-angle X-ray scattering

It is possible to enhance the X-ray scattering yield [35] by matching the energy of X-ray source to a resonant absorption edge in as it is done for resonant inelastic X-ray scattering. Different from standard RIXS measurements, the scattered photons are considered to have the same energy as the incident photons.

SAXS instruments

In a SAXS instrument, a monochromatic beam of X-rays is brought to a sample from which some of the X-rays scatter, while most simply go through the sample without interacting with it. The scattered X-rays form a scattering pattern which is then detected at a detector which is typically a 2-dimensional flat X-ray detector situated behind the sample perpendicular to the direction of the primary beam that initially hit the sample. The scattering pattern contains the information on the structure of the sample. The major problem that must be overcome in SAXS instrumentation is the separation of the weak scattered intensity from the strong main beam. The smaller the desired angle, the more difficult this becomes. The problem is comparable to one encountered when trying to observe a weakly radiant object close to the Sun, like the Sun's corona. Only if the Moon blocks out the main light source does the corona become visible. Likewise, in SAXS the non-scattered beam that merely travels through the sample must be blocked, without blocking the closely adjacent scattered radiation. Most available X-ray sources produce divergent beams and this compounds the problem. In principle the problem could be overcome by focusing the beam, but this is not easy when dealing with X-rays and was previously not done except on synchrotrons where large bent mirrors can be used. This is why most laboratory small angle devices rely on collimation instead. Laboratory SAXS instruments can be divided into two main groups: point-collimation and line-collimation instruments:

Point-collimation instruments

Point-collimation instruments have pinholes that shape the X-ray beam to a small circular or elliptical spot that illuminates the sample. Thus the scattering is centro-symmetrically distributed around the primary X-ray beam and the scattering pattern in the detection plane consists of circles around the primary beam. Owing to the small illuminated sample volume and the wastefulness of the collimation process—only those photons are allowed to pass that happen to fly in the right direction—the scattered intensity is small and therefore the measurement time is in the order of hours or days in case of very weak scatterers. If focusing optics like bent mirrors or bent monochromator crystals or collimating and monochromating optics like multilayers are used, measurement time can be greatly reduced. Point-collimation allows the orientation of non-isotropic systems (fibres, sheared liquids) to be determined.

Line-collimation instruments

Line-collimation instruments restrict the beam only in one dimension (rather than two as for point collimation) so that the beam cross-section is a long but narrow line. The illuminated sample volume is much larger compared to point-collimation and the scattered intensity at the same flux density is proportionally larger. Thus measuring times with line-collimation SAXS instruments are much shorter compared to point-collimation and are in the range of minutes. A disadvantage is that the recorded pattern is essentially an integrated superposition (a self-convolution) of many adjacent pinhole patterns. The resulting smearing can be easily removed using model-free algorithms or deconvolution methods based on Fourier transformation, but only if the system is isotropic. Line collimation is of great benefit for any isotropic nanostructured materials, e.g. proteins, surfactants, particle dispersion and emulsions.

SAXS instrument manufacturers

SAXS instrument manufacturers include Anton Paar, Austria; Bruker AXS, Germany; Hecus X-Ray Systems Graz, Austria; Malvern Panalytical. the Netherlands, Rigaku Corporation, Japan; Xenocs, France; and Xenocs, United States.

See also

Related Research Articles

<span class="mw-page-title-main">Crystallography</span> Scientific study of crystal structures

Crystallography is the experimental science of determining the arrangement of atoms in crystalline solids. Crystallography is a fundamental subject in the fields of materials science and solid-state physics. The word crystallography is derived from the Ancient Greek word κρύσταλλος, with its meaning extending to all solids with some degree of transparency, and γράφειν. In July 2012, the United Nations recognised the importance of the science of crystallography by proclaiming that 2014 would be the International Year of Crystallography.

<span class="mw-page-title-main">X-ray crystallography</span> Technique used for determining crystal structures and identifying mineral compounds

X-ray crystallography is the experimental science determining the atomic and molecular structure of a crystal, in which the crystalline structure causes a beam of incident X-rays to diffract into many specific directions. By measuring the angles and intensities of these diffracted beams, a crystallographer can produce a three-dimensional picture of the density of electrons within the crystal. From this electron density, the positions of the atoms in the crystal can be determined, as well as their chemical bonds, crystallographic disorder, and various other information.

In X-ray crystallography, wide-angle X-ray scattering (WAXS) or wide-angle X-ray diffraction (WAXD) is the analysis of Bragg peaks scattered to wide angles, which are caused by sub-nanometer-sized structures. It is an X-ray-diffraction method and commonly used to determine a range of information about crystalline materials. The term WAXS is commonly used in polymer sciences to differentiate it from SAXS but many scientists doing "WAXS" would describe the measurements as Bragg/X-ray/powder diffraction or crystallography.

<span class="mw-page-title-main">Small-angle neutron scattering</span>

Small-angle neutron scattering (SANS) is an experimental technique that uses elastic neutron scattering at small scattering angles to investigate the structure of various substances at a mesoscopic scale of about 1–100 nm.

<span class="mw-page-title-main">X-ray scattering techniques</span>

X-ray scattering techniques are a family of non-destructive analytical techniques which reveal information about the crystal structure, chemical composition, and physical properties of materials and thin films. These techniques are based on observing the scattered intensity of an X-ray beam hitting a sample as a function of incident and scattered angle, polarization, and wavelength or energy.

<span class="mw-page-title-main">Neutron diffraction</span> Technique to investigate atomic structures using neutron scattering

Neutron diffraction or elastic neutron scattering is the application of neutron scattering to the determination of the atomic and/or magnetic structure of a material. A sample to be examined is placed in a beam of thermal or cold neutrons to obtain a diffraction pattern that provides information of the structure of the material. The technique is similar to X-ray diffraction but due to their different scattering properties, neutrons and X-rays provide complementary information: X-Rays are suited for superficial analysis, strong x-rays from synchrotron radiation are suited for shallow depths or thin specimens, while neutrons having high penetration depth are suited for bulk samples.

<span class="mw-page-title-main">Synchrotron light source</span> Particle accelerator designed to produce intense x-ray beams

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<span class="mw-page-title-main">Biological small-angle scattering</span>

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<span class="mw-page-title-main">Grazing-incidence small-angle scattering</span>

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<span class="mw-page-title-main">Asymmetric flow field flow fractionation</span>

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Frank Steven Bates is an American chemical engineer and materials scientist. Bates is a Regent's Professor (2007–present), a Distinguished McKnight University Professor (1996–present), and department head (1999-2014) in the department of chemical engineering and materials science at the University of Minnesota, where he has been a faculty member since 1989. Prior to his appointment at the University of Minnesota, Bates was a member of the technical staff at AT&T Bell Laboratories from 1982-1989.

<span class="mw-page-title-main">Spin echo small angle neutron scattering</span> Measure of structures from around 20 to 2000 nm in size

Spin echo small angle neutron scattering (SESANS) measures structures from around 20 to 2000 nm in size. The information is presented as a real-space as opposed to a reciprocal space mapping. This can simplify the interpretation for some systems. SESANS is useful for studying processes that occur over relatively long time scales, as data collection is often slow, but large length scales. Aggregation of colloids, block copolymer micelles, Stöber silica particles being a prime examples.

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References

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  35. ↑ Schuelke, Winfried (21 June 2007). Electron Dynamics by Inelastic X-Ray Scattering. Oxford University Press. ISBN   9780191523281.
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