DE102008008829B4 - Method and device for registration of real structure information in massive crystal bodies by means of X-radiation - Google Patents

Abstract

Method for registering real-structure information in massive crystal bodies by means of X-radiation (31), wherein the crystal bodies (5, 51, 52) have a minimum thickness (D) dependent on the ordinal number, with at least one microfocus X-ray tube (2) Crystal body holder (9) and a detector (7) with a detector receiving surface (71) existing device (1) in a natural atmosphere,
wherein a radiation of the crystal body (9) in the crystal body (5, 51, 52) for generating a radiographic shadow image on the detector (7, 71) for registration of the macroscopic real structure (13, 13 ') of the crystal body (5) is carried out,
characterized,
that linear brake beam interferences (14, 15, 14 ', 15', 14 '', 15 '') which can be registered on the detector receiving surface (71) for representing a crystallographic real structure of the solid crystal body (5, 51, 52) by a primary beam (31) with hard X-ray braking radiation (20) in a wavelength range of Δλ ≈ 1.0 to 1.3 λ _min , from which the massive crystal body (5, 51, 52) filters out the exact wavelength (λ) required for diffraction at its lattice planes, ...

Description

The The invention relates to a method and a device for registration of real-structure information in massive crystal bodies by means of X-rays, being the crystal bodies one dependent on the atomic number Have minimum thickness, the device at least one of Microfocus X-ray tube, one Crystal body mount and a detector with a detector receiving surface in a natural the atmosphere exists, with a radiation of the in the crystal body holder located crystal body to generate a radiographic shadow image on the detector to register the macroscopic real structure of the crystal body.

In The industry is working on the macroscopic and / or Crystallographic defect structure of massive crystal bodies, the as single crystals or as coarsely crystalline, out of a few crystallites existing bodies, especially in the form of components are formed with as possible to analyze little effort to quality assurance of the manufactured body bring about.

Under The macroscopic defect structure generally becomes voids and cracks, but also intentionally introduced cavities or additional body understood while the crystallographic defect structure a statement about deviations the real structure of the ideal structure of a crystal body allows.

in the The first case will be classical X-ray radiographic imaging in the form of an X-ray inspection with film, image plate or solid state detector or computed tomography used. For crystallographic analysis the crystal body come z. As the single-crystal diffractometry, the Laue method, the Weissenberg method, the rotary crystal method as well as other methods of use. In the semiconductor industry if necessary, the long topography is added.

The conventional Laue method is an X-ray diffraction method which polychromatic X-ray radiation used in the form of Bremsstrahlung. In the diffraction on the single crystal body punctate Reflexes that receive so-called Laue spots. Location and shape of the Spots are here indicators for the crystallographic real structure evaluation.

The Problems of the Laue method can be best described using the example of exam of single-crystal turbine blades. The same applies to the investigation the goodness of similar ones Components or bred Crystalline bodies.

The Investigations of components such. B. turbine blades are in more elaborate Fashion done in such a way that for example by means of X-rays in the direction of return and with an area detector the component for registering the Laue interference first on the front and then on the back or at the same time "worn down." Lage- and Geometry changes of Laue points have to constantly be evaluated.

The Real structure information statement is not convincing, as the locations of the Defects can not be assigned to the corresponding locations in the bodies and not because of the low information depth of Laue interference the entire crystal volume can be detected. By the two-sided Recording is a high material and time required.

The High energy synchrotron diffraction methods and neutron diffraction techniques also very expensive.

As a high-energy fine-focused electron beam on a Copper Einkristallkugel Shot in high vacuum and in radiation the intensity of X-rays is detected on a film is already by Determann, H .: About the directional distribution the X-ray brake radiation a massive anticode, Ann. Physics 30, 1937, p 481 described. It shows lines and bands, those with the Kikuchi images of electron beam interference comparable to those of Determann, H .: Kikuchi tapes with X-rays, Writings of natural science. Company, Danzig, 1938 are.

In similar The results are aimed at by Wolf, H.-Ch .: Grid source interference hard X-ray bremsstrahlung, Ann. Physics 6th Series, Volume 13, 1953, pp. 381-403, wherein therein with an imaging device lattice source interference with Hard X-ray braking radiation reached and this also an electron beam in a high vacuum is used.

The Problems of both solutions consist in that by the use of electron beams in the High vacuum with the described devices no massive crystal body Air are tested can.

Brummer, O .: The production of "Kikuchi lines and bands" with relatively soft X-rays and the influence of crystal disturbances on this X-ray - Interferences, Z. Naturforschg. 13a, 1958, pp. 571-572. It does not mention an X-ray micrograph and is not visible on the corresponding images.

• a) Es ist eine Strahlungsquelle mit genügend kleinem Brennfleck vorgesehen.
• b) Es ist ausdrücklich eine charakteristische Röntgenstrahlung bei einer Energie von 5 keV bis 20 keV für die gleichzeitige Belichtung der Weitwinkelinterferenzen einzusetzen.
• c) Die Dicke D der Kristalle muss der zur Anwendung kommenden charakteristischen Röntgenstrahlung so angepasst sein, dass sich Interferenzen genügend stark vom Untergrund abheben.
• d) Die Öffnung des Röntgenstrahlenkegels ist groß genug auszubilden, damit auch die Weitwinkelinterferenzen auftreten und registriert werden können.

A combination of the generation of wide-angle interference with a radiographic image is by Brummer, O .: On the simultaneous generation of X-ray interference and the X-ray shadow image of crystals, Z. Naturforschung. 15a, 1960, pp. 875-879. The prerequisites for generating the X-ray interference shadow (RIS) diagrams are the following factors:

• a) It is provided a radiation source with a sufficiently small focal spot.
• b) It is expressly a characteristic X-ray radiation at an energy of 5 keV to 20 keV for the simultaneous exposure of the wide-angle interference use.
• c) The thickness D of the crystals must be adapted to the characteristic X-ray radiation used in such a way that interferences stand out sufficiently strongly from the ground.
• d) The opening of the X-ray cone is large enough to form, so that the wide-angle interference occur and can be registered.

In this is used for the simultaneous generation of X-ray interference and the X-ray shadow image of crystals expressly working only with characteristic radiation, which causes problems which consist in that the sample thickness D due to the absorption preferably thin (D ≤ 50 microns to 300 microns) can be selected so that the interference still stands out against the ground and can be registered. Furthermore it is necessary to choose the anode material accordingly.

One Another problem is that thicker components and in particular massive bodies accordingly thinned Need to become, whereby the process is no longer carried out non-destructive can.

by virtue of the fact stated in the technical articles is simultaneous Picture accumulation for thick and massive crystal body in the subsequent period has not been followed by the professional world.

A device for producing wide-angle reflectance recordings with characteristic X-radiation is in the DD 242 688 A1 The apparatus for investigating small crystal body regions serves to characterize crystallites in terms of orientation, lattice constants, real structure and anisotropic stresses. In this case, in the beam path of an electron beam, a cup which is open toward the electron beam source and is closed with respect to the crystal body with a metal foil is arranged.

A similar device for making wide-angle X-ray reflectance is in the DE 101 18 573 C1 described.

in the In the case of synchrotron beam diffraction methods, it is expedient to use the crystal body time consuming To scan in layers, which is comparable to a tomography is. An application of multi-beam interference is also eliminated because it is the investigation of partially strongly disturbed real crystals is.

Neutron interference shots in radiation have the problem that they are not so highly spatially resolved, about a real structure statement in staggered form over the to hit the entire thickness of the crystal.

A method and apparatus for testing the crystallographic quality of objects having a crystal structure by excitation of Kikuchi pseudo lines in the environmental sphere are disclosed in U.S. Pat DE 690 03 270 T2 described. The method relates to the production of an image of Kikuchi pseudo-lines of a monocrystalline structure with a photon beam. The device has an X-ray generator with a maximum of 0.1 mm microfocus and a structural unit which has in succession a luminous force amplifier, a video recorder or an image receiver and a movable support for the objects to be tested, wherein the support is arranged between the microfocus and the luminous intensity amplifier ,

One Problem is that an image of Kikuchi pseudo lines from diffracted electrons, regardless of the exciting type of photon. It becomes an x-ray tube for Generation of X-ray photoelectrons used in the object that interfere and the Kikuchi pseudo lines produce. The to be tested crystal body must obviously be rotated several times in other angular positions to a new Image "to get. An implementation of the process - production of electrons in the object - is in the direction of radiation only on very thin objects or exclusively on Surfaces possible.

It is a method for radiographic inspection of an object with a crystal lattice in the US Pat. No. 6,295,335 B1 described. It includes steps for diffracting the object with electromagnetic radiation to obtain a radiographic image of the object on a display device. The display device according to an exposure contains the radiographic image composing one the picture is. This image results from a relative displacement of the object. The displacement makes it possible to reproduce the object at a significant attenuation of the parasitic elements, which result from diffraction of the electromagnetic radiation at the crystal lattice of the object. An intensity-enhancing collimator and a postfilter element are used.

One Problem then is that the method exclusively the Improvement of radiography is used. The by fluorescence excitation generated secondary radiation in the crystalline object becomes in the sense of radiographic mapping as disturbing - as "parasitic element "- denotes and the method shows a possibility the damping.

Another method of detecting absorption, refraction and scattering patterns of an object by independently analyzing, registering, digitizing and combining the images is described in U.S.Pat WO 98/16817 A1 The images reach an upper and a lower angular position of a "rocking curve" of a crystal analyzer An x-ray beam generated by a conventional device may be passed to either a Bragg-type crystal analyzer or a Laue-type crystal analyzer Absorbance, refraction, and scattering effects are detected on an optical disk and then digitized, and the digitized images are simultaneously resolved, preferably on a pixel-by-pixel basis, to obtain a combined visible image, which analyzes a "rocking curve." The device contains the crystal analyzer for this purpose.

One The problem is that the method is used to detect diffraction and scattering patterns, the method for improving exclusively a radiographic Figure serves by known scattering effects such as small angle and Compton scattering be kept low and so a radiographic contrast enhancement entry. An illustration of the crystallographic real structure done not, because no diffraction effect is used.

• 1. Bereitstellen eines Strahlbündels einer harten Strahlung,
• 2. Einbringen eines asymmetrischen Einkristall-Monochromators in den Strahlengang, wobei das daran reflektierte Strahlbündel ein flächenförmiges Strahlbündel einer im Wesentlichen parallel gerichteten, aber leicht divergierenden Strahlung ist, die einen spezifischen Divergenzwinkel besitzt,
• 3. Durchstrahlen des Objektes mit dem flächenförmigen Strahlbündel, so dass die Strahlung durch das Objekt hindurchgeht,
• 4. Einbringen eines Kristall-Analysators in den Strahlengang strahlabwärts des Objektes an eine Position, in der die Braggsche Reflexion des flächenförmigen Strahlbündels wirksam ist, das auf den Kristall-Analysator auftrifft, um das Strahlbündel zu beugen und ein gebeugtes Strahlbündel und ein durchgelassenes Strahlbündel zu bilden, wobei die Anordnung so ist, dass der Winkelbereich der Reflexion von den wirksamen Kristallflächen des Analysators um den exakten Braggschen Reflexionswinkel herum zumindest zweimal so groß ist wie der Divergenzwinkel des flächenförmigen Strahlbündels, das durch den Einkristall-Monochromator gebildet wird, und
• 5. Registrieren des gebeugten Strahlbündels oder sowohl des durchgelassenen als auch des gebeugten Strahlbündels an einem punktsensitiven Strahldetektor.

Another method of obtaining an image of an internal structure of an object is in U.S. Patent Nos. 4,149,359 DE 692 28 285 T2 described, wherein the method comprises the following steps:

• 1. providing a beam of hard radiation,
• 2. introducing an asymmetric monocrystal monochromator into the beam path, the beam reflected therefrom being a sheet-like beam of substantially parallel, but slightly divergent, radiation having a specific divergence angle,
• 3. irradiating the object with the sheet-like beam, so that the radiation passes through the object,
• 4. placing a crystal analyzer in the beam path downstream of the object to a position in which the Bragg reflection of the sheet-like beam is incident on the crystal analyzer to diffract the beam and add a diffracted beam and a transmitted beam the arrangement being such that the angular range of the reflection from the effective crystal faces of the analyzer about the exact Bragg reflection angle is at least twice the divergence angle of the sheet-shaped ray formed by the single crystal monochromator, and
• 5. Register the diffracted beam or both the transmitted and the diffracted beam at a point-sensitive beam detector.

One The problem is that the source is an X-ray source with continuous Radiation is used, however, to generate the diffraction interference asymmetric single crystal monochromators both before and after the object that uses the discrete wavelengths needed for diffraction Steer the object and parallelize the X-ray. Farther is a radiographic through the use of monochromators Picture of the object to be examined impossible.

Furthermore, an X-ray topography system in the US 2003/0108152 A1 described, wherein the system includes an X-ray tube, which generates X-rays, which on a limited area of an object, for. B. a silicon wafer act. A detector is arranged to capture the beam after transmission through the object or after reflection on the object. The detector has an array of pixels adapted to the beam surface to produce a digital image on said restricted area. A relative incremental shift between the x-ray tube and the object produces a series of digital images that are combined together. In optional embodiments, x-ray optics are incorporated to create a parallel beam to avoid image duplication, or the effect of image duplication is eliminated by software.

One problem is that the X-ray beam is not shot perpendicularly but at an angle of less than 90 ° to the object. Furthermore, the beam is parallelized after exiting the tube by the subsequent X-ray optics. The parallel beam is trapped by a beam stopper after passing through the object and deflected and directed at a certain angle to the detector. Furthermore, it is necessary in the method and apparatus to perform relative movements between the object and the source to obtain the desired result images. This is an X-ray topography method.

A method and apparatus for testing single crystal objects by means of radioactive irradiation are disclosed in US Pat DE 34 39 471 A1 in which essentially a gamma diffractometer for the investigation of objects in material-technical terms, in particular for the tester of single-crystal vanes for turbomachines is given. The objects are irradiated by the radiation of a gamma source, the intensity profile of a diffracted reflection is recorded with a fixed detector and the half-width of the reflex is measured.

The Device is designed in the manner of a diffractometer and contains in a radiation protection a radioactive gamma source, wherein connected to the protective jacket is a collimator, wherein means for the temporary Outlet of a focused beam on the turntable arranged to be tested Subject are provided and wherein the turntable a fixed Radiated detector and a control and / or evaluation associated are.

One Problem is that first the intensity profile of a reflex. To capture all the reflexes is an object movement by the angle α necessary. The result is a diffraction peak diagram. For its inclusion is a high component and assembly costs required.

A non-destructive analysis method and associated analyzer are disclosed in U.S.Patent US 2004/0196957 A1 which are capable of obtaining a high-contrast image within an object easily and in a manner by shifting when an object is irradiated with homogeneous, collimated X-rays.

One Problem is that the device with parallel rays is working. The object is a crystal for the parallelization of the radiation upstream. The x-ray does not hit the object vertically. The radiation is after passage sent through the object through an analysis crystal before the so affected radiation hits on the detector.

The Problems of the above methods are that none with a single procedure the macroscopic and crystallographic Real structure by obtaining volume information in compact form crystalline bodies and components simultaneously and without any movement of the device components allowed to image using hard bremsstrahlung.

Of the The invention is therefore based on the object, a method and a device for registering real structure information in massive crystal bodies by means of X-radiation to be specified such that the real structure of massive crystal bodies non-destructive, at the same time, displayed quickly and largely visually visible and an immediate assessment the real structure for X-ray microscopic and crystallographic characterization can be made. there especially in the interior of the massive crystal body the crystallographic defects as well as the location and extent of at Defects hollowed out in the production, embedded foreign particles as well as intended cavities as well as crystal body changes can be detected reproducibly and evaluated after loading.

The The object is achieved by a method and a device having the features of the claims 1 and 10 solved.

• - Einsetzen einer unmittelbar hinter dem Strahlaustritt der Mikrofokus-Röntgenröhre angeordneten Blende, deren Blendenloch einen zur Einstellung einer Strahldivergenz ausgebildeten Durchmesser hat,
• – Einstellung eines Abstandes R₂ zwischen dem Kristallkörper und der Detektoraufnahmefläche, wobei der Abstand R₂ mindestens das Zwanzigfache der Entfernung R₁–R₂ des Kristallkörpers vom Strahlaustritt der Mikrofokus-Röntgenröhre beträgt,
• – Einstellung der Belichtungszeit t der Mikrofokus-Röntgenröhre, wobei die eingestellte Belichtungszeit t von der Ordnungszahl des Materials des Kristallkörpers, von der Dicke D des Kristallkörpers und von der Empfindlichkeit des Detektors abhängt, und
• – Einstellung der Beschleunigungsspannung U der Mikrofokus-Röntgenröhre, die eine Intensität des Primärröntgenstrahls erzeugt, bei der die Intensität des Maximums des Primärröntgenstrahls durch die Absorption des Kristallkörpers um mindestens 25% verringert ist, wobei ein gewünschtes Verhältnis zwischen der die radiographische Schattenabbildung erzeugenden Reststrahlintensität und der Interferenzstrahlintensität erreicht und somit ein registrierfähiges Kontrastbild zeitgleich zwischen den Interferenzlinien und der radiographischen Schattenabbildung herbeigeführt wird.

The method for registering real-structure information in X-ray massive crystal bodies, wherein the crystal bodies have a minimum thickness D dependent on atomic number, is provided with a device comprising at least a microfocus X-ray tube, a crystal body holder, and a detector having a detector receiving surface realizes a natural atmosphere, wherein a radiation of the crystal body located in the crystal body holder for generating a radiographic shadow image on the detector for registration of the macroscopic real structure of the crystal body is performed,
in which
line-shaped brake beam interferences that can be registered on the detector mounting surface to represent a crystallographic real structure of the massive crystal body by a primary beam with hard X-ray braking radiation in a wavelength range of Δλ ≈ 1.0 to 1.3 λ _min , from which the massive crystal body exactly the required wavelength for diffraction at its network planes λ, wherein the line-shaped brake beam interferences simultaneously superimpose the radiographic shadow image generated by a remaining residual beam intensity, registering the line-shaped brake beam interferences by means of the following steps:

• - Inserting an arranged immediately behind the beam exit of the microfocus X-ray tube aperture, the aperture hole one for setting has a diameter formed of a beam divergence,
• Setting a distance R ₂ between the crystal body and the detector receiving surface, wherein the distance R _{2 is} at least twenty times the distance R ₁ -R _{2 of} the crystal body from the beam exit of the microfocus X-ray tube,
• Adjustment of the exposure time t of the microfocus X-ray tube, wherein the set exposure time t depends on the atomic number of the material of the crystal body, on the thickness D of the crystal body and on the sensitivity of the detector, and
• Adjusting the acceleration voltage U of the microfocus X-ray tube, which generates an intensity of the primary X-ray beam, wherein the intensity of the maximum of the primary X-ray beam is reduced by at least 25% by the absorption of the crystal body, wherein a desired ratio between the residual beam intensity generating the radiographic shadow image and the Interference beam intensity is achieved and thus a registerable contrast image is brought about at the same time between the interference lines and the radiographic shadow image.

The Irradiation is done with hard X-ray brake radiation in an energy range from 50 keV to 450 keV.

to simultaneous image overlay of the Shadow picture and the brake jet interference lines to one registered enabled Contrast image is for the microfocus X-ray tube a Exposure time t set in minutes range.

Optional can predetermined crystal regions of the crystal body by means of an xy manipulator unit at the crystal body Retaining crystal body holder scanned become.

To increase the imaging overlay on the surface of the detector, adjustment of the distance R _{1 of} the detector relative to the microfocus X-ray tube can be performed by a distance adjusting device.

When massive crystal bodies can monocrystalline or coarsely crystalline crystal bodies are used.

The solid crystal bodies may have a minimum thickness D in the range of a few millimeters to a few centimeters, wherein the introduced into the device and the minimum thickness D having crystal body of the hard X-ray braking radiation of the range of Δλ ≈ 1.0 to 1.3λ _min the exact diffractive wavelength to filter out the line-shaped brake jet interferences yourself.

at Radiation of coarsely crystalline, consisting of single crystals crystalline bodies the aperture serves in combination with a crystal body movement by means of the xy manipulator unit of probing and imaging of Single crystals.

parts the diffraction cone for line-shaped brake jet interference, the outside of the superimposed with interference lines Silhouette exist exclusively contain the information of the crystallographic Real structure in contrast to the diffraction cones in the contrast image, the radiographic shadow illustration and the crystallographic real structure Both diffraction cone types register simultaneously on the detector receiving surface become.

• – eine Mikrofokus-Röntgenröhre, die einen direkten Primärröntgenstrahl mit harter Röntgenbremsstrahlung in einem Energiebereich von 50 keV bis 450 keV liefert,
• – eine Kristallkörper-Halterung zur Halterung des zu untersuchenden Kristallkörpers,
• – einen Detektor mit einer Detektoraufnahmefläche, die in einem Abstand R₁ vom Strahlaustritt der Mikrofokus-Röntgenröhre aus entfernt angeordnet ist, wobei der Kristallkörper zur Erzeugung einer radiographischen Schattenabbildung auf dem Detektor zur Registrierung der makroskopischen Realstruktur des Kristallkörpers durchstrahlt wird,

wobei im Kennzeichenteil des Patentanspruchs 10
zur Erzeugung von registrierfähigen linienförmigen Bremsstrahlinterferenzen auf der Detektoraufnahmefläche unmittelbar hinter dem Strahlaustritt der Mikrofokus-Röntgenröhre und dem gehalterten Kristallkörper eine Blende zur Reduktion seitlicher Streustrahlung sowie zur Strahldivergenzeinstellung angeordnet ist, wobei die Blende mit einem Lochdurchmesser im Millimeterbereich versehen ist, dass ein Abstand R₂ zwischen dem Kristallkörper und der Detektoraufnahmefläche eingestellt ist, der zumindest das Zwanzigfache der Entfernung R₁–R₂ des Kristallkörpers vom Strahlaustritt der Mikrofokus-Röntgenröhre beträgt, und dass eine Beschleunigungsspannung U der Mikrofokus-Röntgenröhre eingestellt ist, die eine Strahlintensität nach dem Kristallkörper erzeugt, bei der die Intensität des Maximums des Primärröntgenstrahls durch die Absorption des Kristallkörpers um mindestens 25% bezüglich des zugehörigen Intensitätsmaximums verringert ist, wodurch ein Verhältnis zwischen der die radiographische Schattenabbildung erzeugenden Reststrahlintensität und der Interferenzstrahlintensität eingestellt ist, mit dem ein auf der Detektoraufnahmefläche registrierfähiges Kontrastbild zwischen Interferenzlinien und radiographischer Schattenabbildung anzeigbar ist.A device for registering real-structure information in massive crystal bodies with X-radiation, wherein the crystal bodies have a minimum thickness D dependent on the atomic number, in a natural atmosphere for carrying out the aforementioned method

• A microfocus X-ray tube providing a direct primary x-ray beam with hard X-ray braking radiation in an energy range from 50 keV to 450 keV,
• A crystal body holder for holding the crystal body to be examined,
• A detector having a detector-receiving surface, which is arranged at a distance R ₁ from the beam exit of the microfocus X-ray tube, wherein the crystal body is irradiated for generating a radiographic shadow image on the detector for registration of the macroscopic real structure of the crystal body,

wherein in the characterizing part of claim 10
for generating registerable line-shaped Bremsstrahlinterferenzen on the detector receiving surface immediately behind the beam exit of the microfocus X-ray tube and the Erten crystal body a diaphragm for reducing lateral scattered radiation and for Strahldivergenzeinstellung is arranged, wherein the aperture is provided with a hole diameter in the millimeter range that a distance R ₂ between is set to the crystal body and the detector receiving surface which is at least twenty times the distance R ₁ -R _{2 of} the crystal body from the beam exit of the microfocus X-ray tube, and that an acceleration voltage U of the microfocus X-ray tube is set to produce a beam intensity after the crystal body the intensity of the maximum of the primary X-ray beam by the absorption of the crystal body by at least 25% with respect to the associated Intensi is reduced maximum, whereby a ratio between the radiographic shadow image generating residual beam intensity and the interference beam intensity is adjusted, with which a recordable on the detector receiving surface contrast image between interference lines and radiographic shadow image can be displayed.

The Aperture is made of a highly absorbent material.

The Aperture can do that be a lead aperture.

Besides that is a lead sheet on the back of the Detector arranged for shielding.

A connected to the microfocus X-ray tube Control device is available, which is used to set the exposure time t to carry out the simultaneous image overlay to the registerable Contrast image and for setting the acceleration voltage U of Microfocus X-ray tube is used.

The Crystal body holder for the crystal body is optionally equipped with an xy manipulator unit, around all given areas of the crystal body in the registry to include and / or single crystallites in the study of coarsely crystalline crystal bodies to probe.

Of the Detector can be an x-ray film, a solid state detector, an image plate or a screen / CCD camera unit.

To avoid an over-radiation of the image centers at the shortest distance R ₁ to the microfocus X-ray tube and at the same time the impact of the primary X-ray residual intensity can optionally be introduced into the beam path of the primary X-ray beam between the crystal body holder and the detector, an absorption filter.

The Absorption filter may be a geometrically formed body, preferably a hemisphere or a sphere segment.

A the filter associated with the absorption filter can from a used X-ray low-absorbent material, preferably carbon fiber-reinforced plastic, so that the image overlay the recording too the recordable Contrast image not disturbed becomes.

The non-destructive method is explained in more detail below:
During the direct transmission, an enlarged radiographic shadow image (for example a defect structure) and the registration of a diffraction information (crystallographic parameters) z. B. a few millimeters to a few centimeters thick and large-area crystal body simultaneously imaged in a shot and performed with exposure times t in the minute range by means of microfocus X-ray tube.

Accordingly, the X-ray beam of the microfocus X-ray tube is used, which is directed through a directly arranged at the beam exit lead aperture on the immediately following, monocrystalline or coarse crystalline, valid as a test sample crystal body. The microfocus X-ray tube uses its hard bremsstrahlung. At a distance R ₁ , whose magnitude may be from a few millimeters to several 100 millimeters, away from the beam exit of the microfocus X-ray tube, there is a detector, for. As an X-ray film, which is shielded at its rear with a lead sheet. Instead of the X-ray film, alternatively, a corresponding solid state detector or an image plate can be used. The crystal body holder can optionally be supplemented by an xy manipulator unit to remove all areas of interest of the crystal body, which may be desirable for larger test samples.

The process management begins with the switching of the said radiation source, z. B. microfocus X-ray tube, in lower minute range. The associated and accurate exposure times t hang from the ray energy, the atomic number of the crystal material, the crystal body thickness and the detector sensitivity.

On the said way become simultaneously adjustable on the detector enlarged X-ray shadow micrograph as well as linear brake jet interference of the irradiated crystal body area in the form of the registerable Contrast image accumulated.

The method is based on the use of hard X-ray brake radiation just above the wavelength λ _min , for example in the wavelength range of Δλ ≈ 1.0 to 1.3 λ _min , and does not use the longer wavelength characteristic radiation of an X-ray tube. The massive crystal body "filters" and monochromatizes to a certain extent even the wavelength required for diffraction at its lattice planes from the continuous brake spectrum Δλ.

The invention enables a nondestructive combination method, which in direct radiation and at the same time an enlarged radiographic shadow image for determining the macroscopic defect structure and the registration of a diffraction information by means of lines shaped Bremsstrahlinterferenzen to determine crystallographic parameters thicker, in particular a few millimeters to a few centimeters thick and large-scale, massive crystal body simultaneously in a recording uses.

The Invention allows because no electron beam with vacuum conditions is needed, the investigation in air and thus also on larger and massive crystal bodies representing Components.

Around all areas of interest or areas of the crystal body or of the component, the crystal body can optionally be "scanned" with the xy manipulator unit.

One another advantage over the frequently used Laue method (surface analysis up to approx. 300 μm Depth) is that the position of the defects in the inventive method on the total crystal body thickness D traced back can be.

Around the procedural overexposure of the Image centers in the shortest Distance to the X-ray source and at the same time at the point of impact of the primary X-ray residual intensity to avoid, can optionally a gradient absorption filter, e.g. B. a hemisphere or a spherical segment, in the X-ray path additionally be introduced. In order that the presentation is not in addition to to disturb, can do that needed Filter holder device from a used X-ray radiation low-absorbent material (eg carbon fiber reinforced plastic) consist.

The inventive method provides real-time information about the total crystal body thickness in the transmission direction and over a larger crystal area.

The inventive method is subject to severe restrictions in industrial testing practice, that the crystal body thickness D as a result of absorption as possible thin (D ≤ 50 microns to 300 microns) can be selected must not, as it is in contrast takes the opposite route, based on the use of hard X-ray braking radiation based and thick, massive crystal bodies in the form of samples or Components in their total crystal body thickness D of a nondestructive Makes the investigation accessible.

Essential is the use of hard X-ray brake radiation in the energy range from 50 keV to 450 keV for direct transmission massive crystal body for simultaneous image overlay a radiographic shadow image for registration of the macroscopic defect structure of the crystal body and a generation of linear Bremsstrahlinterferenzen for registration of the crystallographic Defect structure of the crystal body on a detector for visual or scanning related evaluation.

The Invention allows it that the limitations mentioned in the prior art in terms of be bypassed to be irradiated thickness of the crystal body, since the Method in the range of high energies between 50 keV to about 450 keV and thus in the area of hard X-ray braking radiation is working.

As a result, can also thick and massive components can be examined radiographically.

The to carry out The method of the method is based on an embodiment closer by means of several drawings explains Further, examples of X-ray images obtained by the method are shown specified.

It demonstrate:

1 Representations of the device for registration of real structure information in massive crystal bodies by means of hard X-ray braking radiation on an X-ray film, wherein

1 a schematic representation of the device and

1b an intensity (I) X-ray wavelength (λ) curve with the X-ray brake radiation range used according to the invention
are,

2 an evaluable and recordable contrast image recording according to the invention on an X-ray film of a massive NiAl crystal body with the two image areas - radiographic shadow image and brake beam interference lines - of the registerable contrast image,

3 a schematic representation of real structure information on an X-ray film of a massive TbNi ₂ B ₂ C crystal body with macroscopic pores (voids) and without crystal defects,

4 a schematic representation of real structure information on an X-ray film of a massive TbNi ₂ B ₂ C crystal body with local defects in a lattice plane -. B. a Kleinwinkelkorngrenze - and without macroscopic pores,

5 a real picture of the real structure information on a solid TbNi ₂ B ₂ C crystal body by means of hard X-ray brake radiation after the radiation,
in which

5a a picture of the crystal body with voids and interference lines and

5b an enlarged section of the picture in 5a represent the same crystal body,

6 a schematic representation of real structure information on a single-crystal turbine blade of CMSX-6 without macroscopic pores (voids) and without crystal defects,

7 a schematic representation of real structure information on a single crystal turbine blade of CMSX-6 without macroscopic pores (voids) and with disturbances in the crystal structure - with increased dislocation density - and

8th a real-time acquisition of real-structure information by means of hard X-ray brake radiation on a single-crystal turbine blade made of CMSX-6 without macroscopic pores (voids) and with crystal defects - with increased dislocation density.

• – eine Mikrofokus-Röntgenröhre 2, die einen direkten Primärröntgenstrahl 31 mit harter Röntgenbremsstrahlung 20 in einem Energiebereich von 50 keV bis 450 keV liefert,
• – eine Kristallkörper-Halterung 9 zur Halterung des zu untersuchenden Kristallkörpers 5, 51, 52,
• – einen Detektor 7 mit einer Detektoraufnahmefläche 71, die in einem Abstand R₁ vom Strahlaustritt 21 der Mikrofokus-Röntgenröhre 2 aus entfernt angeordnet ist, wobei der Kristallkörper 5, 51, 52 zur Erzeugung einer radiographischen Schattenabbildung auf dem Detektor 7 zur Registrierung der makroskopischen Realstruktur 13, 13' des Kristallkörpers 5, wie in 3 gezeigt ist, durchstrahlt wird.

The following are the 1 with the 1a . 1b considered together. In 1 . 1a is a device 1 for the registration of real structure information in massive crystal bodies 5 . 51 . 52 represented, which have a minimum thickness D dependent on the atomic number, shown in a natural atmosphere, wherein the device 1 includes

• - A microfocus X-ray tube 2 that have a direct primary x-ray 31 with hard X-ray braking radiation 20 in an energy range from 50 keV to 450 keV,
• - a crystal body holder 9 for holding the crystal body to be examined 5 . 51 . 52 .
• - a detector 7 with a detector receiving surface 71 which emerges from the jet at a distance R ₁ 21 the microfocus X-ray tube 2 is located away from, wherein the crystal body 5 . 51 . 52 to generate a radiographic shadow image on the detector 7 to register the macroscopic real structure 13 . 13 ' of the crystal body 5 , as in 3 is shown, is irradiated.

According to the invention for the production of registerable line-shaped, in the 2 to 8th shown brake jet interference 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' on the detector receiving surface 71 immediately behind the jet exit 21 the microfocus X-ray tube 2 and the salient crystal body 5 . 51 . 52 a panel 4 for reducing lateral scattered radiation and for setting a beam divergence 6 introduced, with the aperture 4 provided with a hole diameter in the millimeter range,
wherein a distance R ₂ between the crystal body 5 . 51 . 52 and the detector receiving surface 71 is set and at least twenty times the distance R ₁ -R _{2 of} the crystal body 5 . 51 . 52 from the beam exit 21 the microfocus X-ray tube 2 is, and
wherein an acceleration voltage U of the microfocus X-ray tube 2 is set, which has a beam intensity after the crystal body 5 . 51 . 52 generated at which the intensity of the maximum of the primary x-ray beam 31 by the absorption of the crystal body 5 . 51 . 52 is reduced by at least 25% with respect to the associated intensity maximum, whereby a ratio between the residual beam intensity generating the radiographic shadow image 3 and the interference beam intensity is set with the one on the detector receiving surface 71 registrable in 2 shown contrast image 30 between interference lines 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' and radiographic shadow illustration 13 . 13 ' can be displayed.

The on the detector receiving surface 71 registrable linear brake jet interference 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' to illustrate the crystallographic real structure of the massive crystal body caused by hard X-ray brake radiation 20 in an in 1b shown wavelength range of Δλ ≈ 1.0 to 1.3λ _min , from which the massive crystal body 5 . 51 . 52 filters out the wavelength λ required exactly for diffraction at its network planes.

In 2 is a recordable contrast image 30 on a detector receiving surface 71 for a NiAl crystal body. In the middle area 22 The image overlay is both the radiographic shadow image and the crystallographic real structure in the form of the line-shaped Bremsstrahlinterferenzen as a registerable contrast image 30 illustrated, wherein on the detector receiving surface 71 at the edge 23 Parts of the diffraction cone 6 '' in continuation of the superimposed Bremsstrahlinterferenzen the contrast image 30 are registered, which contain only the crystallographic real structure.

In the 1 shown aperture 4 consists of a highly absorbent material and represents a lead aperture.

A lead sheet 8th can on the back 10 of the detector 7 be arranged for shielding.

It's one to the microfocus X-ray tube 2 connected control device 17 present for setting the exposure time t for performing the simultaneous image superposition and for adjusting the acceleration voltage U of the microfocus X-ray tube 2 serves.

A crystal body holder 9 is for the massive crystal body 5 . 51 . 52 provided, which optionally with an xy manipulator unit 11 is equipped to all predetermined areas of the crystal body 5 . 51 . 52 to include in the registry and / or to probe single crystallites in the study of coarsely crystalline crystal bodies.

The detector 7 . 71 may be an X-ray film, a solid-state detector, an optical disk or a fluorescent screen / CCD camera unit.

To avoid over-radiation of the image centers at the shortest distance R ₁ to the microfocus X-ray tube 2 and at the same time at the point of impact of the primary X-ray residual intensity optionally an absorption filter (not shown net) in the beam path of the primary X-ray beam 31 between the crystal body holder 9 and the detector 7 . 71 be introduced.

The Absorption filter may be a geometrically formed body, preferably a hemisphere or a sphere segment.

A the filter associated with the absorption filter can from a used X-ray low-absorbent material, preferably carbon fiber-reinforced plastic, so that the accumulation of the recording for the registerable contrast image not disturbed becomes.

The method for registration of real structure information in massive crystal bodies with an X-ray 31 , where the crystal bodies 5 . 51 . 52 have a dependent of the atomic number minimum thickness D, with the aforementioned device 1 at least from a microfocus X-ray tube 2 , a crystal body holder 9 and a detector 7 with a detector receiving surface 71 exists, is realized in a natural atmosphere, with a radiation of the in the crystal body holder 9 located crystal body 5 . 51 . 52 to generate a radiographic shadow image on the detector 7 . 71 to register the macroscopic real structure 13 . 13 ' of the crystal body 5 . 51 . 52 is carried out.

• – Einsetzen einer unmittelbar hinter dem Strahlaustritt 21 der Mikrofokus-Röntgenröhre 2 angeordneten Blende 4, deren Blendenloch 12 einen zur Einstellung einer Strahldivergenz 6 ausgebildeten Durchmesser hat,
• – Einstellung eines Abstandes R₂ zwischen dem Kristallkörper 5, 51, 52 und der Detektoraufnahmefläche 71, wobei der Abstand R₂ mindestens das Zwanzigfache der Entfernung R₁–R₂ des Kristallkörpers 5, 51, 52 vom Strahlaustritt 21 der Mikrofokus-Röntgenröhre 2 beträgt,
• – Einstellung der Belichtungszeit t der Mikrofokus-Röntgenröhre 2, wobei die eingestellte Belichtungszeit t von der Ordnungszahl des Materials des Kristallkörpers 5, 51, 52, von der Dicke D des Kristallkörpers 5, 51, 52 und von der Empfindlichkeit des Detektors 7, 71 abhängt, und
• – Einstellung der Beschleunigungsspannung U der Mikrofokus-Röntgenröhre 2, die eine Intensität des Primärröntgenstrahls 31 erzeugt, bei der die Intensität des Maximums des Primärröntgenstrahls 31 durch die Absorption des Kristallkörpers 5, 51, 52 um mindestens 25% verringert ist, wobei ein gewünschtes Verhältnis zwischen der die radiographische Schattenabbildung erzeugenden Reststrahlintensität 3 und der Interferenzstrahlintensität erreicht und somit ein registrierfähiges Kontrastbild 30 zeitgleich zwischen den Interferenzlinien und der radiographischen Schattenabbildung herbeigeführt wird.

According to the invention on the detector receiving surface 71 registrable line-shaped brake jet interference 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' to show a crystallographic real structure of the massive crystal body 5 . 51 . 52 through a primary beam 31 with hard X-ray braking radiation 20 in a wavelength range of Δλ ≈ 1.0 to 1.3λ _min , from which the massive crystal body 5 . 51 . 52 which filters out exactly to the diffraction required at its network levels wavelength λ generates, with the line-shaped Bremsstrahlinterferenzen 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' by a remaining residual beam intensity 3 overlaying generated radiographic shadow image simultaneously, wherein registration of the line-shaped brake beam interference 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' by means of the following steps:

• - Inserting one immediately behind the jet outlet 21 the microfocus X-ray tube 2 arranged aperture 4 , whose aperture hole 12 one for setting a beam divergence 6 has trained diameter,
• - Setting a distance R ₂ between the crystal body 5 . 51 . 52 and the detector receiving surface 71 wherein the distance R _{2 is} at least twenty times the distance R ₁ -R _{2 of} the crystal body 5 . 51 . 52 from the beam exit 21 the microfocus X-ray tube 2 is,
• - Setting the exposure time t of the microfocus X-ray tube 2 , wherein the set exposure time t of the atomic number of the material of the crystal body 5 . 51 . 52 , of the thickness D of the crystal body 5 . 51 . 52 and the sensitivity of the detector 7 . 71 depends, and
• - Adjustment of the acceleration voltage U of the microfocus X-ray tube 2 giving an intensity of the primary x-ray 31 generated at which the intensity of the maximum of the primary x-ray beam 31 by the absorption of the crystal body 5 . 51 . 52 is reduced by at least 25%, with a desired ratio between the residual beam intensity producing the radiographic shadow image 3 and reaches the interference beam intensity and thus a registerable contrast image 30 at the same time between the interference lines and the radiographic shadow image is brought about.

Irradiation with hard X-ray braking radiation 20 is carried out in an energy range from 50 keV to 450 keV.

For simultaneously mapping the shadow image and the brake beam interference lines to the registerable contrast image 30 is for the microfocus X-ray tube 2 set an exposure time t in the minute range.

Optionally, predetermined crystal regions of the crystal body 5 . 51 . 52 by means of an xy manipulator unit 11 at the crystal body 5 . 51 . 52 retaining crystal body holder 9 be scanned.

To increase the image overlay on the surface 71 of the detector 7 can by a distance adjustment (not shown net) a setting of the distance R _{1 of} the detector 7 . 71 relative to the microfocus X-ray tube 2 be performed.

As a massive crystal body 5 . 51 . 52 Monocrystalline or coarsely crystalline crystal bodies can be used, the crystal bodies 5 . 51 . 52 have a minimum thickness D in the range of a few millimeters to a few centimeters.

In a radiation of coarsely crystalline, consisting of single crystals crystal bodies 5 . 51 . 52 serves the aperture 4 in combination with a crystal body movement by means of the manipulator unit 11 the probing and imaging of single crystals.

The parts of the diffraction cone 6 '' that are outside the diffraction cone 6 ' of the contrast image 30 at the edge 23 the contrast picture 30 contain only the information of the crystallographic real structure, in contrast to the diffraction cones 6 ' in contrast 30 containing the radiographic shadowing and the crystallographic real structure, both diffraction cone types 6 ' . 6 '' simultaneously on the detector receiving surface 71 can be registered.

The use of hard X-ray braking radiation 20 in the energy range from 50 keV to 450 keV
for the simultaneous imaging overlay of information of massive crystal bodies 5 . 51 . 52 having a minimum thickness D dependent on atomic number, in a natural atmosphere according to the method and the apparatus,
by direct irradiation to generate a radiographic shadow image for registration of the macroscopic real structure 13 . 13 ' of the massive crystal body 5 . 51 . 52 and
by means of a generation of shading contrasting, registerable contrast having Bremsstrahlinterferenzlinien for registration of the crystallographic real structure 16 . 14 '' . 15 '' of the massive crystal body 5 . 51 . 52 on a detector 7 and for visual or scanning related evaluation.

The method begins with the turning on of said X-ray source, a microfocus X-ray tube 2 , in the lower minute range.

One to the microfocus X-ray tube 2 connected control device 17 is for setting the exposure time t for performing the simultaneous image superposition.

In the manner described are on the detector 7 . 71 simultaneously an enlarged X-ray shadow microscopy image as well as by diffraction cone 6 ' . 6 '' in the 1a marked X-ray brake beam interference of the irradiated crystal body region of the solid crystal body 5 . 51 . 52 can be registered.

To carry out the method according to the invention is from the microfocus X-ray tube 2 delivered hard X-ray brake radiation 20 used as in the in 1 . 1b illustrated X-ray spectrum 18 contained and in contrast to the characteristic radiation used in the prior art 19 is shown.

The 3 shows a schematic representation of real structure information on an X-ray film 71 from a massive TbNi ₂ B ₂ C crystal body 51 with macroscopic pores (voids) 13 . 13 ' and without crystal defects.

In this case, inside the TbNi ₂ B ₂ C crystal body 51 microscopic cavities 13 . 13 ' or voids are shown as a form of the macroscopic defect structure. The lines of brake radiation interference 14 . 15 on the other hand, as a form of the crystallographic real or defect structure, recorded simultaneously in transillumination, become sharp and uninterrupted next to and through the microscopic voids 13 . 13 ' represented through. This means that the inner surfaces of the cavities 13 . 13 ' are occupied by atoms that attach to the bulk material without crystal defects in the form of the crystallographic defect structure. In this case, it would have to turn on the inside of the TbNi ₂ B ₂ C crystal body 51 to close existing defects, a comparison of pycnometric density measurements with X-ray over a precision lattice constant determination specific density no physically correct result. The device according to the invention 1 does not have these limitations and provides all relevant data, most of which are already visually visible.

The 4 shows a schematic representation of real structure information on the X-ray film 71 from a massive TbNi ₂ B ₂ C crystal body 51 with local crystal defects and without macroscopic pores. The sharp interference lines 14 . 15 but have an interference line break 16 on, the local defects in a lunar system - z. B. a Kleinwinkelkorngrenze - in massive TbNi ₂ B ₂ C crystal body 51 , indicates.

The 5 shows real images of the real structure information according to the inventive method after irradiation by means of hard X-ray braking radiation on the massive TbNi ₂ B ₂ C crystal body 51 , in which 5a a picture of the TbNi ₂ B ₂ C crystal body 51 with voids 13 and interference lines 14 . 15 (strengthened) and 5b an enlarged section of the picture in 4a same TbNi ₂ B ₂ C crystal body 51 with the enlarged blower 13 and the interference 14 . 14 and 14 ' . 15 ' (both highlighted). The crystal body thickness D of the TbNi ₂ B ₂ C crystal body 51 is for example 5 mm and the diameter of the pictures in 5a and 5b imaged crystal body area is 9 mm.

The 6 shows a schematic representation of real structure information on a single crystal turbine blade 52 from CMSX-6 without macroscopic pores (voids) and no crystal disruption, with the absence of crystal disruption leading to sharp interference lines 14 . 15 leads.

The 7 shows a schematic representation of real structure information on the same single-turbine turbine blade 52 from CMSX-6 without macroscopic pores (voids) and with disturbances in the crystal structure - with increased dislocation density -, which in the admission as blurred interference lines 14 '' . 15 '' (Band interferences) are shown.

The 8th shows a real recording of real structure information according to the inventive method after irradiation by means of hard X-ray braking radiation 20 on the single-crystal turbine blade 52 from CMSX-6 without macroscopic pores (voids), but with crystal disruption - with increased dislocation density - due to the blurred interference lines 14 '' . 15 '' are displayed as already in 7 is shown schematically.

The method is used for nondestructive characterization of the quality of massive crystal bodies 5 . 51 . 52 , which are associated with metals, semiconductors, intermetallic compounds, organic crystals and ionic crystals.

The method is based on the use of hard X-ray braking radiation just above the wavelength λ _min , for example in the wavelength range of Δλ ≈ 1.0 to 1.3 λ _min , and does not use the longer wavelength characteristic radiation of an X-ray tube. The massive crystal body 5 . 51 . 52 "Filters" and monochromatizes to a certain extent even the wavelength λ required for diffraction at its network planes from the continuous brake spectrum Δλ.

Especially of massive silicon ingot as starting material for wafers microelectronics and solar technology, piezocrystals, single crystal turbine blades and alloy crystal bodies can the real structure information is determined by registering the simultaneous map accumulation and immediately either visually or through a high-resolution scan be evaluated. But not only related to defect structures, but also in extension to an intended internal education the crystal body can in the massive crystal bodies specifically dimensioned and drawn from the melt cavities and / or while the melt predisposed body on their training, their Location as well as their defects are checked within the crystal body.

Claims (19)

Method for registering real-structure information in massive crystal bodies by means of X-radiation ( 31 ), whereby the crystal bodies ( 5 . 51 . 52 ) have a minimum thickness (D) dependent on the atomic number, with at least one microfocus X-ray tube ( 2 ), a crystal body holder ( 9 ) and a detector ( 7 ) with a detector receiving surface ( 71 ) existing device ( 1 ) in a natural atmosphere, wherein a radiation of the in the crystal body holder ( 9 ) located crystal body ( 5 . 51 . 52 ) for generating a radiographic shadow image on the detector ( 7 . 71 ) for the registration of the macroscopic real structure ( 13 . 13 ' ) of the crystal body ( 5 ), characterized in that on the detector receiving surface ( 71 ) registrable line-shaped brake beam interference ( 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' ) to illustrate a crystallographic real structure of the massive crystal body ( 5 . 51 . 52 ) by a primary jet ( 31 ) with hard X-ray braking radiation ( 20 ) in a wavelength range of Δλ ≈ 1.0 to 1.3 λ _min , from which the massive crystal body ( 5 . 51 . 52 ) which filters out exactly the wavelength (λ) required for the diffraction at its network planes, whereby the line-shaped brake beam interferences ( 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' ) by a remaining residual beam intensity ( 3 ) superimposed radiographic shadow image simultaneously, wherein a registration of the line-shaped Bremsstrahlinterferenzen ( 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' ) is brought about by means of the following steps: - inserting one immediately behind the jet outlet ( 21 ) of the microfocus X-ray tube ( 2 ) arranged aperture ( 4 ), whose aperture hole ( 12 ) one for setting a beam divergence ( 6 ) has a diameter formed, - setting a distance (R ₂ ) between the crystal body ( 5 . 51 . 52 ) and the detector receiving surface ( 71 ), wherein the distance (R ₂ ) at least twenty times the distance (R ₁ -R ₂ ) of the crystal body ( 5 . 51 . 52 ) from the jet outlet ( 21 ) of the microfocus X-ray tube ( 2 ), - adjustment of an exposure time (t) of the microfocus X-ray tube ( 2 ), wherein the set exposure time (t) of the ordinal number of the material of Crystal body ( 5 . 51 . 52 ), of the thickness (D) of the crystal body ( 5 . 51 . 52 ) and the sensitivity of the detector ( 7 . 71 ), and - adjustment of the acceleration voltage (U) of the microfocus X-ray tube ( 2 ) containing an intensity of the primary x-ray beam ( 31 ), at which the intensity of the maximum of the primary x-ray beam ( 31 ) by the absorption of the crystal body ( 5 . 51 . 52 ) is reduced by at least 25%, wherein a desired ratio between the residual beam intensity generating the radiographic shadow image ( 3 ) and the interference beam intensity and thus a registerable contrast image ( 30 ) is caused at the same time between the interference lines and the radiographic shadow image. Method according to claim 1, characterized in that the irradiation of the crystal bodies ( 5 . 51 . 52 ) with hard X-ray braking radiation ( 20 ) is performed in an energy range of 50 keV to 450 keV. A method according to claim 1, characterized in that for the simultaneous image superposition of the shadow image and the Bremsstrahlinterferenzlinien to registerable contact image ( 30 ) for a microfocus X-ray tube ( 2 ) an exposure time (t) in the minute range is set. Method according to one of claims 1 to 3, characterized in that optionally predetermined crystal regions of the crystal body ( 5 . 51 . 52 ) by means of an xy manipulator unit ( 11 ) at the crystal body ( 5 . 51 . 52 ) holding crystal body holder ( 9 ) are scanned. Method according to one of claims 1 to 4, characterized in that to increase the image overlay on the surface ( 71 ) of the detector ( 7 ) by means of a distance adjusting device, an adjustment of the distance (R ₁ ) of the detector ( 7 . 71 ) relative to the microfocus X-ray tube ( 2 ) is carried out. Method according to one of claims 1 to 5, characterized in that as massive crystal body ( 5 . 51 . 52 ) monocrystalline or coarsely crystalline crystal bodies are used. Process according to claim 6, characterized in that the crystal bodies ( 5 . 51 . 52 ) have a minimum thickness (D) in the range of a few millimeters to a few centimeters. A method according to claim 6 or 7, characterized in that when irradiated by coarsely crystalline, consisting of single crystals crystal bodies ( 5 . 51 . 52 ) the aperture ( 4 ) in combination with a crystal body movement by means of the xy manipulator unit ( 11 ) of probing and imaging of single crystals. A method according to claim 1, characterized in that parts of the diffraction cone ( 6 '' ) for linear brake jet interference ( 32 ) outside the contrast image ( 30 ) at the edge ( 23 ) of the recording, the diffraction cones ( 6 '' ) contain exclusively the information of the crystallographic real structure, in contrast to the diffraction cones ( 6 ' ) in the contrast image ( 30 ), the radiographic shadow image and the crystallographic real structure in the registerable contrast image ( 30 ), both diffraction cone types ( 6 ' . 6 '' ) simultaneously on the detector receiving surface ( 71 ). Contraption ( 1 ) for registration of real structure information in massive crystal bodies by means of X-radiation ( 31 ), whereby the crystal bodies ( 5 . 51 . 52 ) have a minimum thickness (D) dependent on atomic number, in a natural atmosphere, for carrying out a method according to one of claims 1 to 9, comprising - a microfocus X-ray tube ( 2 ) providing a direct primary x-ray ( 31 ) with hard X-ray braking radiation ( 20 ) in an energy range from 50 keV to 450 keV, - a crystal body holder ( 9 ) for holding the crystal body to be examined ( 5 . 51 . 52 ), - a detector ( 7 ) with a detector receiving surface ( 71 ), which at a distance (R ₁ ) from the beam exit ( 21 ) of the microfocus X-ray tube ( 2 ) is removed from, wherein the crystal body ( 5 . 51 . 52 ) for generating a radiographic shadow image on the detector ( 7 ) for the registration of the macroscopic real structure ( 13 . 13 ' ) of the crystal body ( 5 ) is irradiated, characterized in that for the generation of registerable line-shaped Bremsstrahlinterferenzen ( 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' ) on the detector receiving surface ( 71 ) immediately behind the jet exit ( 21 ) of the microfocus X-ray tube ( 2 ) and the salient crystal body ( 5 . 51 . 52 ) an aperture ( 4 ) for the reduction of lateral scattered radiation and for setting a beam divergence ( 6 ), wherein the diaphragm ( 4 ) is provided with a hole diameter in the millimeter range, that a distance (R ₂ ) between the crystal body ( 5 . 51 . 52 ) and the detector receiving surface ( 71 ), which is at least twenty times the distance (R ₁ -R ₂ ) of the crystal body ( 5 . 51 . 52 ) from the jet outlet ( 21 ) of the microfocus X-ray tube ( 2 ), and that an acceleration voltage (U) of the microfocus X-ray tube ( 2 ), which has a beam intensity after the crystal body ( 5 . 51 . 52 ), at which the intensity of the maximum of the primary x-ray beam ( 31 ) by the absorption of the Kristallkör pers ( 5 . 51 . 52 ) is reduced by at least 25% with respect to the associated intensity maximum, whereby a ratio between the residual beam intensity generating the radiographic shadow image ( 3 ) and the interference beam intensity is adjusted, with the one on the detector receiving surface ( 71 ) recordable contrast image ( 30 ) between interference lines ( 14 . 15 . 14 . 15 ' . 14 '' . 15 '' ) and radiographic shadow image ( 13 . 13 ' ) can be displayed. Device according to claim 10, characterized in that the diaphragm ( 4 ) consists of a highly absorbent material. Device according to claim 11, characterized in that the diaphragm ( 4 ) is a lead aperture. Apparatus according to claim 10, characterized in that a lead sheet ( 8th ) on the back side ( 10 ) of the detector ( 7 ) is arranged for shielding. Apparatus according to claim 10, characterized in that a to the microfocus X-ray tube ( 2 ) connected control device ( 17 ) for adjusting the exposure time (t) for performing the simultaneous image overlay to the registerable contrast image (16). 30 ) and for adjusting the acceleration voltage (U) of the microfocus X-ray tube ( 2 ) serves. Apparatus according to claim 10, characterized in that the crystal body holder ( 9 ) for the crystal body ( 5 . 51 . 52 ) optionally with an xy manipulator unit ( 11 ) to all predetermined areas of the crystal body ( 5 . 51 . 52 ) and / or to probe single crystallites in the investigation of coarsely crystalline crystal bodies. Apparatus according to claim 10, characterized in that the detector ( 7 . 71 ) is an X-ray film, a solid-state detector, an optical disk, or a screen / CCD camera unit. Device according to one of claims 10 to 16, characterized in that to avoid an over-radiation of the image centers at the shortest distance (R ₁ ) to the microfocus X-ray tube ( 2 ) and at the same time at the point of impact of the primary X-ray residual intensity ( 3 ) an absorption filter in the beam path of the primary x-ray beam ( 31 ) between the crystal body holder ( 9 ) and the detector ( 7 . 71 ) is introduced. Device according to claim 17, characterized in that the absorption filter is a geometrically formed body, preferably a hemisphere or a sphere segment. Device according to claim 17 or 18, characterized in that a filter holder device associated with the absorption filter consists of a material which only slightly absorbs the used X-ray radiation, preferably carbon fiber-reinforced plastic, so that the image superposition during the recording of the registerable contrast image ( 30 ) is not disturbed.