Bednorz-Müller experiment 2026-10-18
In 1986, Johannes Georg Bednorz and Karl Alexander Müller precipitated mixed oxalates from aqueous barium, lanthanum and copper nitrates using oxalic acid. Heating at for five hours preceded pressing at and reheating for sintering. X-ray diffraction resolved three phases. Rectangular pieces carried gold electrodes and indium wires; four-terminal sensing in a continuous-flow cryostat measured electrical resistance versus temperature. Annealing atmosphere and measuring electric current density were varied; larger electric current densities suppressed the drop. An onset near differed from the much lower temperature where the drop approached three orders of magnitude.[ref]
This was evidence for possible granular superconductivity, with phase identification unfinished. The paper deferred Meissner effect and heat capacity tests; its proof note corrected bulk lanthanum/barium ratios. A resistive onset did not establish a uniform bulk superconducting transition temperature.[ref]
Possible high Tc superconductivity in the Ba-La-Cu-O system by Johannes Georg Bednorz and Karl Alexander Müller. §IV, p.192; proof note, p.193
Their 1987 authored lecture describes later magnetometer checks on lead, followed by magnetic susceptibility measurements: samples with a resistive drop developed diamagnetism at somewhat lower temperatures. Combining magnetic, transport and X-ray diffraction results identified barium-substituted as the superconducting phase. These later results strengthened the case beyond the initial mixed-phase transport evidence.[ref]
GaN blue LED development 2026-10-18
Isamu Akasaki chose metalorganic vapour-phase epitaxy and sapphire, which tolerated hot ammonia. Large lattice mismatch hindered film growth. In 1985, Hiroshi Amano and Isamu Akasaki's group developed an aluminium nitride epitaxial buffer layer deposited before hotter gallium nitride growth. The buffer supplies initial growth sites; growing islands join into a continuous film. It improves growth without making the lattices identical. Isamu Akasaki separately credits Shuji Nakamura's 1991 gallium nitride buffer.[ref]
https://www.kapitza.ras.ru/~glazkov/students/Nobel-akasaki-lecture.pdf. §§3.2–4.2, pp. 13–20, Figs. 7–11: growth sequence and microscopy
The 1986 growth paper reports a vertical metalorganic vapour-phase epitaxy reactor, source gases mixed just before delivery to slanted sapphire, and subsequent gallium nitride growth over aluminium nitride. Surface microscopy, X-ray diffraction and photoluminescence tested different aspects of the result. Buffered and unbuffered growth supplied the comparison. Its reported preparation conditions should not be replaced by one universal buffer temperature: the later lecture's account of the first low-temperature trial and the paper's parameter study describe different stages of development.[ref]
Metalorganic vapor phase epitaxial growth of a high quality GaN film using an AlN buffer layer by Hiroshi Amano and others. p. 353, Fig. 1 and Table I; p. 354, surface and diffraction comparisons
A magnesium acceptor impurity in gallium nitride accepts a valence band Electron, leaving a mobile electron hole. Hydrogen passivation of magnesium acceptors in gallium nitride suppresses this activity. Post-growth activation restores existing impurities' electrical activity; ionization of active acceptor impurities supplies mobile electron holes. Adding magnesium alone is insufficient.[ref]
Hole Compensation Mechanism of P-Type GaN Films by Shuji Nakamura and others. p. 1258, abstract and §1: passivation and activation
In 1989, Hiroshi Amano, Masahiro Kito, Kazumasa Hiramatsu and Isamu Akasaki obtained p-type semiconductor conduction in magnesium-doped gallium nitride using low-energy Electron beam irradiation. Hiroshi Amano recalls initially resistive samples, an unreliable hot-probe test, then Masahiro Kito's Hall effect confirmation. A junction irradiated in an M-shaped region emitted in that pattern. Treatment, carrier-sign measurement and spatial emission supplied different evidence. Earlier zinc-doped samples brightened under irradiation without becoming p-type semiconductors: brightness alone did not prove the carrier sign.[ref]
https://journals.aps.org/rmp/pdf/10.1103/RevModPhys.87.1133. §V, pp. 1135–1136, Figs. 3–4; authors of 1989 paper in references, p. 1137
Shuji Nakamura, Takashi Mukai, Masayuki Senoh and Naruhito Iwasa's 1992 thermal-activation paper established another route using annealing in nitrogen. Their companion study compared already conducting films heated in nitrogen with films heated in ammonia: the latter became highly resistive again. Its hydrogen-complex explanation connected this atmosphere dependence to acceptor impurity passivation. These are thermal treatment and atmosphere comparisons, distinct from the earlier Electron beam intervention; neither observation alone images an individual hydrogen complex.[ref]
Thermal Annealing Effects on P-Type Mg-Doped GaN Films by Shuji Nakamura and others. abstract: nitrogen annealing above 700 degrees Celsius and electrical changes
[ref]Hole Compensation Mechanism of P-Type GaN Films by Shuji Nakamura and others. p. 1258, abstract and §§1–2: activation history, nitrogen/ammonia comparison and hydrogenation hypothesis
Shuji Nakamura's two-flow metalorganic chemical vapor deposition reactor, gallium nitride buffer, thermal activation and improved indium gallium nitride growth enabled bright double heterostructure devices, followed by thinner quantum well devices.[ref]
The original 1994 paper by Shuji Nakamura, Takashi Mukai and Masayuki Senoh describes a sapphire/gallium nitride-buffer device with zinc-doped indium gallium nitride emission and aluminium gallium nitride confinement. After nitrogen annealing, etching exposed the n-side for a separate contact. At room temperature, varied forward electric currents gave emission spectra and optical-output curves alongside a current-voltage characteristic. At : output, peak wavelength, terminal electric potential difference. The peak stayed nearly fixed across the current series. The paper omits a complete calibrated collection apparatus; comparisons with earlier devices change several preparation details.[ref]
Candela-class high-brightness InGaN⁄AlGaN double-heterostructure blue-light-emitting diodes by Shuji Nakamura and others. pp. 1687–1688, fabrication and Figs. 1–4
Gasper J. Piermarini 2026-10-18
Laue X-ray diffraction experiment of 1912 2026-10-18
Max von Laue proposed crystal X-ray diffraction and wrote the theoretical section; Walther Friedrich and Paul Knipping performed the experiments.[ref]
Interferenz-Erscheinungen bei Röntgenstrahlen by Walther Friedrich, Paul Knipping and Max von Laue. pp. 303–304, 311: section authorship
An X-ray tube, lead apertures and shielding supplied a narrow beam through a crystal on a goniometer. Photographic plates recorded the direct beam and separate spots. Copper(II) sulfate trials preceded oriented zinc blende. Optical alignment was checked with X-rays. Removing the crystal removed the extra spots; grinding destroyed their ordered arrangement; translation preserved it, while tilt changed it. Rotation about the beam rotated the pattern.[ref]
Interferenz-Erscheinungen bei Röntgenstrahlen by Walther Friedrich, Paul Knipping and Max von Laue. pp. 311–318: apparatus and controls
Spots and orientation dependence supported wave interference and three-dimensional crystal periodicity. They determined neither all atomic positions nor an absolute wavelength scale. The authors left open whether the selected radiation originated as crystal fluorescence or was already in the incident beam. This differs from the modern Laue method.[ref]
Interferenz-Erscheinungen bei Röntgenstrahlen by Walther Friedrich, Paul Knipping and Max von Laue. pp. 310–311, 320–322: inference and spectral uncertainty
The 1914 Nobel Prize in Physics went to Max von Laue; the discovery's experimental account remains jointly credited to Walther Friedrich and Paul Knipping.[ref]
The Nobel Prize in Physics 1914 by Nobel Prize Outreach. 1914 award and laureate
The subsequent inference of particular crystal structures is developed under X-ray crystallography. Nobel Prize in Physics in 1914 2026-10-18
Awarded to Max von Laue for the discovery of X-ray diffraction by crystals.[ref]
The Nobel Prize in Physics 1914 by Nobel Prize Outreach. Official award record: laureate and diffraction subject
Use temperature-dependent X-ray diffraction, with the crystal in a controlled heating stage and a detector measuring diffracted directions. A reflection occurs when the scattering wavevector matches a reciprocal lattice vector, or equivalently when Bragg's law is satisfied. Record peak positions and intensities while heating to infer changes in lattice spacings and structure.
A monatomic conventional BCC cell has nonzero crystal basis structure factor only when is even. For FCC the indices must be all even or all odd. The change in reflection selection and peak positions therefore distinguishes the phases. For instance, BCC starts with a family whereas FCC starts with , when indexed in their own conventional cells.
The transformation can create multiple orientation variants, grains, strain and phase coexistence. A reciprocal point that formerly satisfied the diffraction geometry may disappear or move off a fixed detector; a loss of one spot alone does not identify the new phase. Thermal expansion shifts peaks, thermal motion weakens coherent intensities, and hot iron may oxidize without a protective atmosphere.
After transformation, scan crystal angle and scattering angle or use an area detector to locate the new reflections. If single-crystal order has been lost, powder X-ray diffraction or a sufficiently broad orientation survey collects rings or many grain reflections instead of relying on the original alignment. Index several new peaks using the FCC selection rule and fit their common lattice parameter; this probes the new structure even when the original crystal orientation is no longer usable.
To determine a crystal structure, scatter probes whose wavelength is comparable to atomic spacings, typically . X-ray diffraction, neutron diffraction and electron diffraction probe periodic order through coherent elastic scattering. With incident and outgoing wavevectors , define . Elastic scattering has and constructive interference occurs when , a reciprocal lattice vector. The equivalent Bragg's law iswhere the detector scattering angle is , not . Peak positions reveal plane spacings and the unit cell; systematic absent reflections constrain centring and the atomic basis.
For X-ray diffraction, a laboratory tube or a synchrotron supplies a collimated beam. In a monochromatic single-crystal experiment a goniometer rotates the specimen and an area detector records reflection positions and integrated wave intensities. A powder experiment uses many randomly oriented crystallites; the reflections form cones recorded as rings or peaks versus , permitting indexing and determination of lattice constants without selecting one crystallite. For a cubic cell, for example, . The white-beam Laue method is especially useful for crystal orientation.
The crystal basis structure factor isafter geometric and thermal corrections, including the Debye–Waller factor. For X-rays, describes scattering from the atomic electron density. Thus positions provide lattice geometry while relative wave intensities constrain atomic positions and species. Wave intensities do not directly give the phases of : structure refinement or other constraints must address the phase problem.
Neutron diffraction uses a reactor or spallation source, wavelength selection and a detector bank or time-of-flight detection. Neutrons interact with nuclei through nuclear scattering lengths that vary between elements and isotopes rather than simply with atomic number. This makes them useful for light atoms, isotope contrast and distinguishing some neighbours in the periodic table; their magnetic interaction also probes magnetic order. Electron diffraction in a transmission electron microscope gives strong signals from very small thin crystallites, although strong multiple scattering often complicates quantitative wave intensity analysis. These techniques complement one another.
A phonon dispersion relation requires both momentum and energy transfer, so elastic diffraction alone is insufficient. In coherent inelastic neutron scattering, the measured transfers for phonon creation areHere is the phonon wavevector reduced into a Brillouin zone, and labels an acoustic phonon branch or optical phonon branch. Negative energy transfer corresponds to annihilating an already occupied phonon. For neutrons , so wavelength and energy selection are linked. Typical thermal-neutron energies of a few to tens of millielectronvolts ( electronvolts) are well matched to many lattice vibrations.
A triple-axis spectrometer uses a monochromator crystal to select , the sample as the second scattering axis, and an analyser crystal to select before detection. Rotate these elements and the specimen to hold fixed while scanning ; inelastic peaks locate . Repeat at different along symmetry directions to map the phonon dispersion relation. The dynamic structure factor governs peak weights, including the selection of phonon polarization by the scattering geometry. A time-of-flight spectrometer instead infers outgoing neutron energy from travel time over a known flight path and records many directions simultaneously.
Inelastic X-ray scattering can also resolve phonons when very high energy resolution is available. Optical Raman scattering and Brillouin scattering measure vibrations near the zone centre because photon momentum transfers are small compared with a typical reciprocal lattice spacing; they complement, rather than generally map the entire zone like, momentum-resolved neutron measurements. Ultrasound measurements give the long-wavelength sound speed, the initial slope of an acoustic phonon branch.
Powder X-ray diffraction 2026-10-18
Powder X-ray diffraction measures X-ray diffraction from many crystal grains with different orientations. For each allowed set of lattice spacings, suitable grains satisfy Bragg's law and produce a cone of diffracted directions, seen as a ring on an area detector or a peak in an angular scan. Several peak positions and systematic absences can identify a crystal structure even when a sample no longer retains one single-crystal orientation. Preferred orientation, strain and phase coexistence can complicate interpretation.
Ruby calibration against sodium chloride 2026-10-18
The 1975 experiment mixed powdered sodium chloride and 0.5%-chromium ruby in a 4:1 volume ratio. An Inconel gasket, initially thick with a hole, held the powder and 4:1 methanol–ethanol. At , X-ray diffraction rings on film away gave salt compression; a reference equation of state assigned pressure. After decreasing load, they waited at least five hours and bracketed diffraction exposures with readings to check drift.[ref]
Calibration of the pressure dependence of the R1 ruby fluorescence line to 195 kbar by Gasper J. Piermarini and others. pp. 2774–2775, Experimental Procedures
The recommended linear slope was , with a fit confidence interval of , to . Reference-scale systematic measurement uncertainty remained separate. Above about the medium was only quasihydrostatic; separate range fits checked consistency.[ref]
Calibration of the pressure dependence of the R1 ruby fluorescence line to 195 kbar by Gasper J. Piermarini and others. pp. 2775–2776, Table I and recommended calibration; p. 2778, pressure-distribution discussion
The logical chain is compression to reference pressure, paired with optical shift, then a fitted response. X-ray diffraction supplies the reference comparison during calibration; subsequent ruby readings transfer that scale to other samples. The reference equation of state is therefore part of the meaning of the reported pressure. Changing it can move all calibrated readings together, even if the optical measurements repeat perfectly. A regression residual tests agreement with the chosen reference within the sampled conditions; it cannot independently certify that reference.
Alongside the 1927 Davisson–Germer experiment, George Paget Thomson developed an independent transmission test. Alexander Reid first used celluloid; Thomson used thin metal films. A narrow Electron beam crossed a film about thick, reaching a photographic plate perpendicular to the beam. Rings appeared. Accelerating voltages of – set the de Broglie wavelengths; metal structures known from X-ray diffraction allowed quantitative comparison. A downstream magnetic field deflected ring-forming Electrons like those passing through holes, identifying the carriers as Electrons rather than X-rays. Celluloid's uncertain structure limited its quantitative interpretation.[ref]
The Davisson–Germer experiment uses crystal reflection and angular electric current scans; this transmission camera records a spatial pattern behind the specimen. Both probe interference in electron diffraction, with different specimen preparations and readouts. A developed photographic plate records accumulated detections, not a direct image of the wavefunction.
Why rings? In an ideal film containing many small crystals with uniformly distributed orientations, a family of lattice planes with spacing can satisfy Bragg's law at every azimuth about the incident beam. First-order elastic scattering then forms a cone of opening half-angle , where . A flat detector a distance downstream cuts this cone in a circle:The last expression requires small scattering angles. It explains a useful control: hold the specimen and camera distance fixed, increase accelerating voltage, and the ring radii should shrink with the electron accelerating-voltage wavelength. It predicts positions, not intensities: preferred crystal orientations, film thickness and repeated quantum scattering can alter a real pattern.
For a chosen example, take and . The exact relativistic electron accelerating-voltage wavelength gives at and at . The corresponding exact ring radii are and . These are calculated examples with chosen spacings and camera distance, not Thomson's measurements. The higher voltage lies outside the range quoted from his lecture, deliberately illustrating a prediction rather than reconstructing his data.
X-ray crystallography 2026-10-18
X-ray crystallography infers a crystal structure from measured X-ray diffraction. Peak positions constrain the lattice geometry, while intensities constrain the atomic basis of a crystal; the inference also needs an experimental model and does not directly observe every atomic position.
X-ray diffraction 2026-10-18
X-ray diffraction is the angular redistribution of X-ray wave intensity through wave interference between scattered waves. In a crystal structure, repeated lattice translations select discrete outgoing directions by the Laue equations. A photographic plate can therefore turn invisible atomic periodicity into a visible constellation of spots. Their geometry constrains the Bravais lattice and its orientation; their wave intensities also depend on the crystal basis structure factor. Determining atomic positions belongs to X-ray crystallography and requires more information than recognizing a spot pattern.
The Laue X-ray diffraction experiment of 1912 established this phenomenon experimentally. The Laue method uses a fixed crystal structure with a range of incident wavelengths; the Bragg crystal reflection experiment of 1913 instead measured angularly resolved signals with a moving detector. These are different ways of finding the same coherent elastic scattering directions.
