DE102007049929A1 - Hollow waveguide used in medicine and in structural analysis comprises a channel structure having an inner coating with a specified thickness - Google Patents

Abstract

Hollow waveguide comprises a channel structure having an inner coating with a thickness of less than 50 nm. An independent claim is also included for a method for the production of the hollow waveguide.

Description

The The invention relates to internally coated hollow optical waveguides especially for guidance, shaping and reinforcement electromagnetic waves or particle radiation are suitable, Process for their preparation and the use of the internally coated Hollow optical fibers.

X-rays plays in various fields of technology, such as medicine, structural analysis and materials science play an important role. It wins because of the desire for increasingly better resolution capabilities analytical systems or after further miniaturization of Structures the use of particularly short-wavelength, hard X-rays more and more important. Therefore, systems are increasingly needed with which such radiation lead, form and strengthen leaves.

For high energy radiation with wavelengths below 100 nm, conventional lenses are not suitable. Instead, become in the art for guiding and shaping such radiation special systems, in particular toroidal concave mirrors, Fresnel zone plates and capillary optics used. Here are facing capillary optics Among other things, the advantages of a technological less expensive and therefore cheaper production, the usability of a larger solid angle range the radiation used and the possibility of flexible Guiding the radiation, for example around obstacles, as needed especially for medical applications becomes.

Indeed is the inherent reflectivity for high energy Radiation in the case of materials such as glass, for example used for the production of hollow fiber waveguides, low. For guidance, shaping and reinforcement, for example of EUV radiation and weak X-rays are therefore internally coated hollow fiber waveguides have been used.

From the US 5,130,172 A For example, a method of metal plating surfaces by chemical vapor deposition or gas phase laser photoablation from a volatile organometallic compound is known.

DE 198 52 722 C1 describes a process for the interior coating of monocapillaries as well as the use of coated monocapillars or bundles of coated monocapillaries for certain catalytic and optical applications.

It However, it has been found that according to the known Method available inner coatings of hollow fiber waveguides insufficient quality for many optical applications exhibit. Due to insufficient X-ray optical properties In particular, such hollow waveguides can not be used for hard X-radiation. Therefore be used for leadership, shaping and reinforcement of Hard X-radiation so far hollow fiber waveguide Leaded glass used. However, it has turned out that such Glasses are very hard to work with and only a short life to have. For example, when using hollow fiber waveguides made of leaded glass for reinforcement of hard X-radiation after 5000 hours of operation compared to the beginning of use measured intensities intensity losses of more than 50% observed.

It There is therefore a need for other systems of leadership, Forming and amplification of electromagnetic waves or Particle radiation, in technical and economic terms have improved usability and in particular also for Use with hard X-radiation are suitable.

These Task is through the internally coated hollow fiber waveguide according to one of claims 1 to 14 and 40 solved. The invention also relates to a Method for producing an internally coated hollow optical waveguide according to claims 15 to 39 and the use of an internally coated hollow waveguide according to a of claims 41 and 42.

Of the Inner coated hollow waveguide according to the invention characterized by having (a) a channel structure and (b) comprises an inner coating on the inner surface of the channel structure, wherein the channel interior facing surface of the Inner coating has a height of less than 50 nm.

invention internally coated hollow optical waveguides have in comparison to known hollow optical waveguides much better optical, especially X-ray optical Properties on. Surprisingly, the are hollow waveguide according to the invention in contrast to known interior coated systems also for guidance, Shaping and amplification of hard X-radiation. They have a significantly improved long-term stability compared to the uncoated used for this purpose Hollow fiber waveguides made of leaded glass.

The term "channel structure" here comprises both monocanal structures and polychannel structures and denotes a structure which consists of one or more spatially arranged at regular intervals, continuous and on consists of the ends of open channels. Examples of mono-channel structures are monocapillaries. Examples of multi-channel structures are polycapillaries, composite lenses made of individual mono- and / or polycapillaries, monolithic lenses made of individual mono- and / or polycapillaries, photonic crystals and monolithic integral microlenses.

Of the Inner diameter of a single channel of the channel structure is usually in the range of 1 nm to 10 mm. The inner diameter is preferred less than 1000 microns, especially less than 100 microns.

For example are generally inside diameters of the channels in compound lenses made of monocapillaries in the range of 1 to 10 mm, monolithic Lenses made of monocapillaries in the range of 0.1 to 1 mm, in compound lenses made of polycapillaries in the range from 10 to 100 μm, produced on monolithic lenses from polycapillaries in the range of 1 to 10 microns and monolithic integral microlenses in the range of 0.3 to 1 μm.

Polycapillaries are usually monolithic structures having a plurality of channels, the channels being substantially equal in length and usually having a length to internal diameter ratio of at least about 100: 1, preferably at least about 1000: 1. Polycapillaries may contain, for example, more than 10 ³ to more than 10 ⁶ channels having internal diameters of, for example, less than 1 mm to less than 1 μm.

Photonic crystals are artificial periodic structures of a dielectric (eg glass) with specific optical properties. In addition to glass, other materials can be used. Photonic crystals are used, for example, in optical metrology, communication technology and the life sciences and are described in VP Bykov, "Spontaneous emission in a periodic structure", Soviet Physics JETP, American Institute of Physics, New York 1972, 35, 269 and in K. Busch et al. (Ed.), "Photonic Crystals Advances in Design, Fabrication, and Characterization", Wiley-VCH, 1st Edition, 2004 ,

monolithic integral microlenses are very largely miniaturized multichannel structures, For example, the channels with inner diameters of about 0.3 to 1 micron can have.

Various mono- and multi-channel structures are commercially available for example from the IFG - Institute for Scientific Instruments GmbH, Berlin-Adlershof, Germany, the universities Antis Europe GmbH, Georgsmarienhütte Germany and the X-Ray Optical Systems, Inc., (XOS ^®), East Greenbush, NY, USA available.

Multi-channel structures often show in direct comparison to their outer wall a relatively thin channel wall on. This channel wall is significantly thinner than the outer wall of Monocapillaries, since it only serves to separate the channels and has no structure-bearing function as in monocapillaries. This is due to their monolithic multichannel structures Forest possible.

In In a preferred embodiment, the channel structure made of an inorganic material or a plastic. To suitable Inorganic materials include carbon, for example nanoporous carbon and carbon nanotubes (CNT), silicon, Glass, ceramics and metal, for example steel and aluminum. Examples for suitable plastics are in particular silicones. Especially Preferably, the channel structure is made of glass. examples for Suitable types of glass are in particular quartz glass, Duranglas and N16B glass, with quartz glass and Duranglas are preferred.

Farther it is preferred that the channel structure heat conducting or contains Wärmeleitdrähte, z. B. by during the production of the channel structure (eg in the drawing process) Metals, in particular heat-conducting wires, in the Channel structure are introduced. This ensures a isotropic temperature distribution within the channel structure, resulting in positive for thermal coating processes (see below) as well on applications of hollow waveguide according to the invention at higher temperatures.

The Inner coating usually contains one of Carbon different element from the second to fifth Main group or a subgroup of the Periodic Table of the Elements. Preferably, the inner coating contains an element selected from the group consisting of Be, Ni, Pt, Cu, Pd, Ag, W, Re, Ir, Os, Au, Pb, Bi and U, where the elements Ni, Ag, Au, W, Pb, Pt, Bi and U are particularly preferred.

In another preferred embodiment the inner coating is a metal with an atomic number Z> 27, in particular Z> 40, most preferably Z> 71.

It is particularly preferred that the inner coating is a metallic Coating is essentially free of other elements, in particular substantially free of carbon.

The inner coating can be, for example consist of metal layers and / or metal particles, more preferably of amorphous metal layers and / or amorphous metal particles, in particular of amorphous metal layers. It is particularly preferred that the inner coating is in the form of a closed layer layer, in particular a Franck-van der Merve growth layer.

The Interior coatings according to the invention are typical very smooth and characterized by low corrugation, in particular due to low rms surface roughness and low height.

Of the Term "corrugation" refers to a measure of the surface finish, which is essentially through the rms surface roughness, the height of the surface and the degree of coverage of the coating is determined. It will low corrugation, in particular due to low rms surface roughness, a low height and a high degree of coverage favors.

Of the Term "rms surface roughness" refers to the root-mean-square roughness of the surface.

Of the Term "height" with respect to a surface here the value at which 95% of the heights of the surface are less than or equal to this value.

Of the Term "degree of coverage" with respect to a coating here the proportion of an area under the coating, which is covered by the coating.

In a preferred embodiment, the channel interior facing surface of the inner coating a rms surface roughness less than 10 nm, especially less than 5 nm, most preferably less than 2 nm. The height of the channel interior facing surface of the inner coating is preferably less than 15 nm, especially less than 8 nm, most preferably less than 4 nm. The degree of coverage of the inner coating is preferably at least 95%, in particular at least 98%, most preferably at least 99%.

If the inner coating is made up of particles, the particles have usually a very narrow particle size distribution on. It is preferred that the particles are monodisperse. Particularly preferably, the inner coating contains particles with a particle size distribution in which the Standard deviation of particle size less than 20%, especially less than 10%, most preferably less than 5% of the mean particle size.

Generally The thickness of the inner coating can vary depending on Inner diameter of the channel structure varies widely become. For example, an inventive Inner coating have a thickness in the range of 1 to 1000 nm. Preferably, the inner coating according to the invention a thickness in the range of 10 to 250 nm, in particular 50 to 150 nm, most preferably 80 to 120 nm. It has shown, that inner coatings of this thickness for optical properties are particularly suitable.

The The invention also relates to a process for the preparation of the invention internally coated hollow fiber waveguides. This process is remarkable characterized in that the inner coating by a photolytic Process (for example laser coating), an electrochemical Method (for example, an electrochemical coating method), a plasma technological process or a gas phase process is deposited in the channel structure.

Examples for gas phase processes are the chemical vapor deposition (CVD), chemical vapor infiltration (CVI) or the physical Vapor deposition (PVD). In particular, methods are suitable where the inner coating by chemical vapor deposition of elemental organic compounds, for example chemical vapor deposition of organometallic compounds (OMCVD), chemical vapor infiltration of elemental organic compounds, for example, chemical vapor infiltration of organometallic compounds (OMCVI), or gas phase epitaxy of organometallic compounds, for example gas phase epitaxy of Organometallic compounds (OMVPE), deposited in the channel structure become. The term "elemental organic compound" refers to here in particular a compound which differs from carbon Element from the second to fifth main group or one Subgroup of the Periodic Table of the Elements as well as organic groups and / or Contains carbonyl which is chemically direct and / or over an element of the fifth or sixth main group to the respective element are bound. Suitable organoelement compounds for In particular, gas-phase processes are also complexes or coordination compounds. which contain an organic ligand and / or carbonyl. there complex or coordination compounds are preferred, the one Ligands selected from the group consisting of carbonyl, Hexafluoroacetylacetonato and acetylacetonato included.

By coating processes in which high temperatures or energies are used, such as by the physical vapor deposition or the chemical vapor deposition, in particular the thin channel wall of multi-channel structures can be destroyed due to the effect of energy. The chemical vapor deposition of organometallic compounds, in particular the chemical vapor deposition of organometallic compounds (OMCVD), a coating method is provided here, with the coatings of channel structures at relatively low temperatures can be carried out without damaging or destroying them.

• (a) Evakuieren der Kanalstruktur, wobei zwischen den Enden der Kanalstruktur ein Druckgradient aufgebaut wird,
• (b) Einstellen der gesamten Kanalstruktur auf eine konstante Temperatur im Bereich von 273 K bis 2073 K, bevorzugt 293 K bis 873 K, am meisten bevorzugt 373 K bis 723 K, die 50 K bis 150 K, bevorzugt 80 K bis 120 K unterhalb der Zersetzungstemperatur des Precursormaterials liegt,
• (c) Verdampfen eines Precursormaterials und Transport des Precursormaterials durch die Kanalstruktur durch den Druckgradienten,
• (d) Abscheiden einer Beschichtung aus dem Precursormaterial durch lokal begrenzte Zufuhr von Energie.

In a preferred embodiment, a method for producing the internally coated hollow waveguides according to the invention comprises the steps

• (a) evacuating the channel structure, establishing a pressure gradient between the ends of the channel structure,
• (b) adjusting the total channel structure to a constant temperature in the range of 273K to 2073K, preferably 293K to 873K, most preferably 373K to 723K, 50K to 150K, preferably 80K to 120K below the decomposition temperature of the precursor material is,
• (c) evaporating a precursor material and transporting the precursor material through the channel structure through the pressure gradient,
• (D) depositing a coating of the precursor material by locally limited supply of energy.

to Implementation of this procedure is first the Channel structure using a temperature-stable adhesive, preferably a two-component adhesive, gas-tightly connected to a vacuum system. Examples of suitable two-part adhesives are Epoxy resin adhesive, which are temperature stable up to about 450 K, and Silicone adhesives that are temperature stable up to about 570 K. In front the further process steps, the adhesive is sufficiently long hardened.

Possibly may before step (a) the inner surface of the channel structure to be activated. This activation of the inner surface For example, by passing molecular oxygen, preferably at a temperature in the range of 480 K to 773 K. By activating the inner surface of their adsorption capacity is clear improves and so the affinity of the coating material increased significantly compared to the inner surface. Therefore, activating the inner surface can also be the Type of growth behavior of the coating on the inner surface influence positively.

Further, prior to step (a) and optionally before activation of the interior surfaces, the channel (s) of the channel structure may be cleaned. This can be done, for example, by plasma treatment, e.g. B. by an inductively or capacitively generated plasma, chemical processes and / or evacuation with simultaneous annealing. In particular, the cleaning of the channel (s) of the channel structure can be effected by evacuation at a pressure below 10 ^-3 mbar with simultaneous annealing, preferably at a temperature in the range of 473 K to 773 K. By cleaning the channel (s), any organic contaminants of the inner surface, above all, can be removed by combustion to carbon dioxide, thus achieving improved adhesion of the inner coating to the inner surface.

In front Step (a), optionally before activating the inner surface (s) and optionally before or after cleaning the channel (s) a thermal smoothing of the inner surface (s) of the channel (s) of the channel structure. Especially can the thermal smoothing of the inner surface (s) of the channel (s) by heating to one Temperature in the range of 473 K to 2073 K, preferably 573 K to 1473 K, the 50 K to 1500 K, especially 100 K to 1000 K, preferably 150 K to 300 K below the softening point of Glass is lying. By thermal smoothing of the inner surface (s) Corrugation of the inner surface can be reduced in particular, the formation of Innenbeschichturigen with low height favored.

For the transport of the precursor material through the channel structure, a pressure gradient is established between the ends of the channel structure. For this, the channel structure is evacuated from one of its ends. In this case, a minimum pressure of less than 10 ^-2 mbar, preferably less than 10 ^-3 mbar and particularly preferably less than 10 ^-4 mbar is set at this end.

Evaporation of the precursor material can be assisted by using a vacuum system in which the channel structure is evacuated from both ends with different vacuum pumps. Such a vacuum system is for example in DE 198 52 722 C1 described.

In contrast, it is preferred according to the invention that the channel structure is evacuated only from one of its ends. Surprisingly, if the channel structure is evacuated only from one of its ends, a more homogeneous flow behavior of the precursor material is achieved. As a result, a Innenbe coating can be obtained, which is characterized by an extremely low height. In addition, in this embodiment, a smaller amount of foreign material, ie material other than the precursor material, in particular a smaller amount of oxygen, transported through the channel structure. As a result, inner coatings of higher quality can be obtained.

Of the Transport of the precursor material through the channel structure may further also supported by an adjustable carrier gas flow become.

Subsequently the entire channel structure is at a constant basic temperature in the range of 273 K to 2073 K, preferably 293 K to 873 K, most preferably 373 K to 723 K set, the 50 K to 150 K, preferred 80 K to 120 K below the decomposition temperature of the precursor material lies. The constant basic temperature can be, for example, by heating or heating with a heater (eg electric heater or Induction furnace) or by coupling electromagnetic waves (eg microwave or infrared radiation).

The Precursor material is vaporized and by the pressure gradient, optionally with the assistance of the carrier gas flow, through transports the channel structure. The precursor stream and optionally the carrier gas stream can be at a defined Preheat temperature, this temperature 50th K to 150 K, preferably 80 K to 120 K below the decomposition temperature of the precursor material lies.

The Deposition of a coating made of the precursor material through locally limited supply of energy. Through this energy supply is set locally a temperature equal to or greater as the decomposition temperature of the precursor material. Prefers becomes a local temperature due to localized supply of energy in the range of 273 K to 2073 K, more preferably 293 K to 873 K, most preferably 423 K to 723 K set. By the decomposition of the precursor material becomes the inner coating on the inner surface the channels deposited.

In In a preferred embodiment, the duration of the supply locally limited energy in step (d) chosen so that an inner coating with a thickness in the range of 10 to 250 nm, especially 50 to 150 nm, most preferably 80 to 120 nm is deposited. Surprisingly, you can through such a simple choice of coating time interior coatings obtained by a particularly low corrugation, low surface roughness and low height distinguished and particularly suitable for optical applications are.

Prefers the localized supply of energy takes place thermally and / or photochemically, in particular by a heat or radiant heater, an oven, a laser, microwave radiation and / or a plasma. In a particularly preferred embodiment takes place the localized supply of energy by combining a thermal and a photochemical supply of energy, in particular by a combination of heating or heating with a heater (eg electric heater or induction furnace) or by coupling electromagnetic waves (eg microwave or infrared radiation) with irradiation (eg with a laser).

The inventive adjustment of the channel structure to a constant base temperature below the decomposition temperature of the precursor material allows it to be coated to reduce necessary local additional energy supply. Surprisingly This can result in a much better controllable deposition behavior of the Interior coating can be realized, the formation of closed Layer layers with extremely low height allows.

Possibly can, by subsequently passing a gas through a chemical, physical and / or morphological change of the coating be effected. Examples of suitable gases are oxygen, Hydrogen or nitrogen. For example, impurities can by combustion, for example from organic radicals to carbon dioxide and water, to be removed.

The Process for the preparation of the inventive internally coated hollow optical waveguide preferably comprises the implementation an in-situ process analysis. Based on process analytics The manufacturing process can be controlled so that special advantageous inner coatings are obtained. A process analysis For example, by optical measurement methods, by online mass spectrometry or by taking gas samples and measuring by gas chromatography respectively.

An in-situ determination of the coating thickness can be carried out in particular by laser transmission. For this purpose, the transmission of laser radiation, for example a red laser with a wavelength range of 660 to 680 nm, in the direct beam passage through the hollow waveguide is determined by measuring the photocurrent caused in a photodiode. The measured photocurrents are corrected on the basis of reference values which are obtained in each case in the same arrangement without a hollow-fiber waveguide or with the uncoated hollow-waveguide. Scanning electron microscopy determined coating thicknesses are with the for the respective Beschich tion thicknesses obtained photocurrents correlated. The correlation thus obtained makes it possible to carry out a non-destructive quantitative determination of the coating thickness in the current coating process and thus to control the production process of the internally coated hollow optical waveguides according to the invention to achieve a specific coating thickness.

A Control of the manufacturing process may also or additionally based on a product analysis of the inventively prepared internally coated hollow optical waveguide. Can do this suitable for carrying out an analysis Preparations are made, for example cross sections using an ultramicrotome for energy-dispersive X-ray measurements, in particular a two-dimensional x-ray mapping, as well for trans-electron microscopy or scanning electron microscopy Investigations. This can be caused by the choice of process parameters Changes in the characteristics of the interior coatings studied and used to further control the manufacturing process become.

In the method of the invention can different precursor materials are used. That's it advantageous if the precursor material is a sublimable material wherein a sublimable material at room temperature is preferred. It is also advantageous if the precursor material is stable with respect to Air is.

Prefers is a precursor material that is an element other than carbon from the second to the fifth main group or a subgroup of the Periodic Table of the Elements as well as organic groups and / or carbonyl contains, directly and / or chemically Element of the fifth or sixth main group to the respective Element are bound. In particular, the precursor material can be a organometallic compound having at least one metal-carbon bond, or a complex or coordination compound having a contains organic ligand and / or carbonyl. There are Complex or coordination compounds which select a ligand are preferred from the group consisting of carbonyl, hexafluoroacetylacetonato and acetylacetonato.

In a preferred embodiment, the precursor material comprises an element selected from the group consisting of Be, Ni, Pt, Cu, Pd, Ag, W, Re, Ir, Os, Au, Pb, Bi, and U, wherein the elements Ni , Ag, Au, W, Pb, Pt, Bi and U are particularly preferred. Particularly preferred is a precursor material which is selected from the group consisting of
Bis (1,1,1,5,5,5-hexafluoro-2,4-pentanedionato) palladium (II),
tetracarbonylnickel,
nickelocene,
2,2,6,6-tetramethyl-3,5-heptanedionatosilber (I),
Tris (2,2,6,6-tetramethyl-3,5-heptanedionato) bismuth (III),
tetraethyl lead,
Bis (2,2,6,6-tetramethyl-3,5-heptanedionato) lead (II),
Uranium hexafluoride,
uranocene,
uranium acetate,
tungsten hexacarbonyl,
Dimethyl (hexafluoroacetylacetonato) gold,
Tetrakis (triphenylphosphine) platinum (0)
Bis (hexafluoroacetylacetonato) platinum (II),
Bis (acetylacetonato) platinum (II),
Dimethyl (1,5-cyclooctadiene) platinum (II),
Methyl (triphenylphosphine) gold (I) and
Bis (1,1,1,5,5,5-hexafluoro-2,4-pentanedionato) -lead (II).

The Invention also relates to internally coated hollow waveguides, which are obtainable by the method described above. Surprisingly, draw the inner coatings of such internally coated hollow optical waveguides through a special surface morphology. Without restriction on a particular theory is assumed to be through the method according to the invention homogeneous layer layers with low corrugation, low surface roughness and low altitude, which are made up of particles, the one monodisperse particle size distribution have and a special, in particular abplatte, in the dimension have upset perpendicular to the coating surface shape. These internally coated hollow optical waveguides are in particular for optical applications advantageous. Preferred embodiments this inner-coated hollow optical waveguide have materials, Coating thicknesses, surface roughness, heights and / or particle size distributions as above Are defined.

The Invention also relates to the use of the invention internally coated hollow fiber waveguides. In particular, it concerns the invention the use of the invention internally coated hollow fiber waveguides for shaping, guiding, Focusing and amplification of electromagnetic waves or particle radiation, in particular of microwaves, wherein the Wavelength range of 100 cm to 1 mm particularly preferred is, of visible light, the wavelength range from 380 to 750 nm is particularly preferred, from UV radiation, wherein the wavelength ranges from 50 to about 190 nm (VUV range) and 1 to 50 nm (EUV range) are particularly preferred, of laser radiation, X-ray and particle radiation (γ-radiation and neutron radiation).

Especially preferred are the low energy range of the X-radiation with an energy of 0.124 to 1.24 keV (corresponding to one wavelength from 1 to 10 nm); the higher energy range of X-rays with an energy of 1.24 to 12.4 keV (corresponding to one wavelength from 0.1 to 1 nm), especially the discrete wavelengths the Cu-Kα radiation (8 keV); and the high energy area the X-radiation with an energy of 12.4 to 124 keV (corresponding to a wavelength of 0.01 to 0.1 nm), in particular the discrete wavelengths of MoKα radiation (17 keV). Particularly preferred is the range of X-radiation with an energy of 15 to 30 keV.

Especially in the high energy range of X-rays is the Wavelength of the radiation to be amplified smaller as the distance of the atoms in the solid state. Surprisingly are the internally coated according to the invention Hollow-waveguide especially for shaping, guidance, Focusing and amplification of electromagnetic waves suitable whose wavelengths are less than the rms surface roughness and / or the height of the channel interior facing surface the inner coating.

Prefers is also the use of the invention internally coated hollow optical waveguides for X-ray lithographic Applications such as Soft X-ray Lithography (SXRL) with 1 to 2 keV or X-ray depth lithography like Deep X-ray Lithography (DXRL) with 4 to 10 keV. Also preferred is the use for X-ray microscopy applications in the spectral range from about 2 to about 4 nm (water window).

One particular advantage of the interior coated according to the invention Hollow fiber optic cable is their improved long-term stability when used for forming, guiding, focusing and Amplification of electromagnetic waves or particle radiation. For uncoated hollow-fiber waveguides, for example made of leaded glass, carry energy recordings, for example by X-ray exposure, long term to material damage to the hollow fiber waveguides and thus to loss of intensity and the uselessness of structures. In the inner coated hollow optical waveguides according to the invention can such material damage is at least largely avoided.

Especially The use according to the invention is preferably also internally coated Hollow-waveguide for focusing EUV radiation or X-radiation for (X-ray) lithographic applications, for example in the mask exposure for semiconductor production. Prefers the use according to the invention is also internally coated Hollow-waveguides in X-ray procedures, especially in X-ray endoscopy.

The The invention will now be discussed in more detail with reference to selected examples explained.

example 1

A 250 mm long fused silica monocrillet, having a length of 250 mm, an outside diameter of 0.8 mm and an inside diameter of 0.55 mm, was gas-tightly connected to a vacuum system by means of a two-part adhesive at one end and heated several times by simultaneous heating to 650 K and passing 1000 mbar molecular oxygen purified from the inside. Subsequently, a constant basic temperature of the polycapillary structure of 373 K was set. The minimum pressure set by the vacuum system was 10 ^-5 mbar. As precursor W (CO) _{6 was} used. By means of a mobile kiln system, a locally limited temperature of 696 K was set in sections over a period of 120 minutes. Finally, the monocapillar structure was sealed under inert gas conditions.

XRD (X-Ray Diffraction) measurements were carried out with the obtained inner coating ( 1 ). No reflections were measured in the relevant areas. This shows that the resulting coating was amorphous.

The coating thickness of the inner coating was determined by scanning electron microscopy to be 104 nm. The surface morphology of the inner coating was investigated by AFM (Atomic Force Microscopy) ( 2 ). These studies confirmed that an inner coating having very little corrugation was obtained. A closer examination revealed that the surfaces had an rms surface roughness of 1 nm and a height of 1-2 nm.

The internally coated monocapillary was examined by means of X-ray optical measurements in an energy range of 15 to 30 keV. Intensity gains of up to more than 80 were achieved ( 3 ).

Example 2

An N16B 250 mm long, 2 mm OD, 0.5 mm I.D. mono capillary was gas tightly attached to a vacuum system by means of a two-part adhesive at one end and heated several times by simultaneous heating to 650 K and passing 1000 mbar molecular oxygen purified from the inside. Subsequently, a constant basic temperature of the polycapillary structure set by 373K. The minimum pressure set by the vacuum system was 10 ^-5 mbar. As precursor W (CO) _{6 was} used. By means of a mobile kiln system, a locally limited temperature of 696 K was set in sections over a period of 120 minutes. Finally, the monocapillar structure was sealed under inert gas conditions.

The internally coated monocapillary was examined by means of X-ray optical measurements in an energy range of 15 to 30 keV. Intensity gains of up to 75 were achieved ( 3 ).

Example 3

A glass polycapillary structure having a length of 50 mm and a maximum outside diameter of 7.20 mm was used which contained about 40,000 channels with a channel internal diameter of 29.5 μm. This polycapillary structure was connected to a vacuum system at one end as in Example 1 and cleaned from the inside. Subsequently, a constant basic temperature of the polycapillary structure of 373 K was set. The minimum pressure set by the vacuum system was 10 ^-5 mbar. As precursor W (CO) _{6 was} used.

By a portable furnace system was over a period of 118 minutes in sections a localized temperature of 723 K set. The supplied via the furnace system Energy as well as the temperature gradient were kept constant.

QUOTES INCLUDE IN THE DESCRIPTION

This list The documents listed by the applicant have been automated generated and is solely for better information recorded by the reader. The list is not part of the German Patent or utility model application. The DPMA takes over no liability for any errors or omissions.

Cited patent literature

• - US 5130172 A [0005]
• - DE 19852722 C1 [0006, 0043]

Cited non-patent literature

• VP Bykov, "Spontaneous emission in a periodic structure", Soviet Physics JETP, American Institute of Physics, New York 1972, 35, 269 [0016]
• K. Busch et al. (Ed.), "Photonic Crystals Advances in Design, Fabrication, and Characterization," Wiley-VCH, 1st Edition, 2004. [0016]

Claims (43)

Internal coated hollow fiber waveguide, the a) a channel structure and b) an inner coating on the inner Surface of the channel structure includes, wherein the Channel interior facing surface of the inner coating has a height of less than 50 nm. Inner-coated hollow-fiber waveguide according to claim 1, in which the channel structure has a mono-channel structure or a multi-channel structure is. Inner-coated hollow-fiber waveguide according to claim 2, in which the monochannel structure is a monocapillary. Inner-coated hollow-fiber waveguide according to claim 2, in which the multi-channel structure is selected from the Group made up of polycapillaries, compound lenses from single mono- and / or polycapillaries, monolithic lenses made of single mono- and / or polycapillaries, photonic Crystals and monolithic integral microlenses. Inner coated hollow fiber waveguide after a of claims 1 to 4, wherein the channel structure made of glass consists. Inner coated hollow fiber waveguide after a of claims 1 to 5, wherein the channel structure Wärmeleitfäden or contains Wärmeleitdrähte. Inner coated hollow fiber waveguide after a of claims 1 to 6, wherein the inner coating a element other than carbon from the second to the fifth Main group or a subgroup of the Periodic Table of the Elements contains. Inner coated hollow fiber waveguide after a of claims 1 to 7, wherein the inner coating a Metal selected from the group consisting of Be, Ni, Contains Pt, Cu, Pd, Ag, W, Re, Ir, Os, Au, Pb, Bi and U, wherein the elements Ni, Ag, Au, W, Pb, Pt, Bi and U are particularly preferred are. Inner coated hollow fiber waveguide after a of claims 1 to 8, wherein the inner coating a Metal with an atomic number Z> 27, in particular Z> 40, most preferably Z> 71 contains. Inner coated hollow fiber waveguide after a of claims 1 to 9, wherein the inner coating of Metal layers and / or metal particles, preferably of amorphous Metal layers and / or amorphous metal particles, in particular from consists of amorphous metal layers. Inner coated hollow fiber waveguide after a of claims 1 to 10, wherein the channel interior facing surface of the inner coating an rms surface roughness less than 10 nm, especially less than 5 nm, most preferably less than 2 nm. Inner coated hollow fiber waveguide after a of claims 1 to 11, wherein the channel interior facing surface of the inner coating a height of less than 15 nm, especially less than 8 nm, most preferably less than 4 nm. Inner coated hollow fiber waveguide after a of claims 1 to 11, wherein the degree of coverage of the Internal coating at least 95, in particular at least 98 most preferably at least 99. Inner coated hollow fiber waveguide after a of claims 1 to 13, wherein the inner coating particles containing a particle size distribution, at the standard deviation of the particle size less than 20, in particular less than 10 most preferred is less than 5% of the mean particle size. Inner coated hollow fiber waveguide after a of claims 1 to 14, wherein the inner coating a Thickness in the range of 1 to 1000 nm, preferably 10 to 250 nm, in particular 50 to 150 nm, most preferably 80 to 120 nm. Process for producing an internally coated Hollow-waveguide according to one of claims 1 to 15, in which the inner coating is produced by a photolytic process, an electrochemical process, a plasma technology process or depositing a vapor phase process in the channel structure. The method of claim 16, wherein the inner coating by chemical vapor deposition (CVD), chemical vapor infiltration (CVI) or Physical Vapor Deposition (PVD) in the channel structure is deposited. The method of claim 17, wherein the inner coating by chemical vapor deposition of Organometallver compounds (OMCVD), Chemical vapor phase infiltration of organometallic compounds (OMCVI) or Gas Phase Epitaxy of Organometallic Compounds (OMVPE) is deposited in the channel structure. The method of claim 17 or 18, comprising the steps (a) evacuating the channel structure, establishing a pressure gradient between the ends of the channel structure, (b) adjusting the total channel structure to a constant base temperature in the range of 273K to 2073K, preferably 293K to 873K, most preferably 373K up to 723 K, which is 50 K to 150 K, preferably 80 K to 120 K below the decomposition temperature of the precursor material, (c) vaporizing a precursor material and transporting the precursor material through the channel structure through the pressure gradient, and (d) depositing a coating from the Precursor material by locally limited supply of energy includes. The method of claim 19, wherein prior to step (a) activates the inner surface (s) of the channel structure become. The method of claim 20, wherein activating the inner surface (s) by passing over molecular Oxygen, preferably at a temperature in the range of 480 K to 773 K, takes place. Method according to one of claims 19 to 21, in which before step (a) and if necessary before activating the In nenoberfläche (n) the channel (s) of the channel structure getting cleaned. The method of claim 22, wherein the cleaning the channel (s) of the channel structure by plasma treatment, chemical processes and / or evacuation with simultaneous annealing takes place. The method of claim 23, wherein the cleaning of the channel (s) of the channel structure by evacuation at a pressure below 10 ^-3 mbar with simultaneous annealing, preferably at a temperature in the range of 473 K to 773 K occurs. Method according to one of claims 19 to 24, in which before step (a), optionally before activation of the inner surface (s) and optionally before or after cleaning the channel (s) a thermal smoothing of the inner surface (s) of the channel (s) of the channel structure. The method of claim 25, wherein the thermal Smoothing the inner surface (s) of the channel (s) Channels of the channel structure by heating to a Temperature in the range of 473 K to 2073 K, preferably 573 K to 1473 K, the 50 K to 1500 K, especially 100 K to 1000 K, preferably 150 K to 300 K below the softening point of Glass is lying. Method according to one of claims 19 to 26, in which the channel structure is evacuated only from one of its ends becomes. Method according to one of claims 19 to 27, wherein in step (a) a minimum pressure of less than 10 ^-2 mbar, preferably less than 10 ^-3 mbar, and more preferably less than 10 ^-4 mbar, is set. Method according to one of claims 19 to 28, in which the transport of the precursor material through the channel structure supported in step (c) by a carrier gas stream becomes. Method according to one of claims 19 to 29, wherein in step (d) a local temperature in the range of 273 K is adjusted to 2073 K, preferably 293 K to 873 K. Method according to one of claims 19 to 30, in which the supply of energy in step (d) is controlled by a heat or radiant heater, an oven, a laser, microwave radiation and / or a plasma takes place. Method according to one of claims 19 to 31, wherein the supply of energy in step (d) by combination a thermal and a photochemical supply of energy takes place. Method according to one of claims 19 to 32, further, the passage of a gas to the chemical, physical and / or morphological change of the coating. Method according to one of claims 19 to 33, the further implementation of an in-situ process analysis and process control. Method according to one of claims 19 to 34, wherein the precursor material is a sublimable material. Method according to one of claims 19 to 35, wherein the precursor material is different from carbon Element from the second to fifth main group or one Subgroup of the Periodic Table of the Elements as well as organic groups and / or contains carbonyl which is chemically direct and / or over an element of the fifth or sixth main group to the respective element are bound. Method according to one of claims 19 to 36, in which the precursor material comprises an organometallic compound, having at least one metal-carbon bond, or a Complex or coordination compound that is an organic ligand and / or carbonyl. A method according to claim 37, wherein the complex or coordination compound selected a ligand from the group consisting of carbonyl, hexafluoroacetylacetonato and acetylacetonato. Method according to one of claims 19 to 38, wherein the precursor material is an element selected from the group consisting of Be, Ni, Pt, Cu, Pd, Ag, W, Re, Ir, Os, Au, Pb, Bi and U, where the elements Ni, Ag, Au, W, Pb, Pt, Bi and U are particularly preferred. Method according to one of claims 19 to 39, in which the precursor material is selected from the group consisting of Bis (1,1,1,5,5,5-hexafluoro-2,4-pentanedionato) palladium (II), tetracarbonylnickel, nickelocene, 2,2,6,6-tetramethyl-3,5-heptanedionatosilber (I), Tris (2,2,6,6-tetramethyl-3,5-heptanedionato) bismuth (III), tetraethyl lead, Bis (2,2,6,6-tetramethyl-3,5-heptanedionato) lead (II), Uranium hexafluoride, uranocene, uranium acetate, tungsten hexacarbonyl, Dimethyl (hexafluoroacetylacetonato) gold, Tetrakis (triphenylphosphine) platinum (0) Bis (hexafluoroacetylacetonato) platinum (II), Bis (acetylacetonato) platinum (II), Dimethyl (1,5-cyclooctadiene) platinum (II), Methyl (triphenylphosphine) gold (I) and Bis (1,1,1,5,5,5-hexafluoro-2,4-pentanedionato) -lead (II). Inner coated hollow fiber waveguide available according to a method according to one of the claims 16 to 40. Use of an internally coated hollow fiber waveguide according to one of claims 1 to 15 or 41 or one according to one of claims 16 to 40 produced internally coated hollow waveguide for Formation, leadership, focus and reinforcement electromagnetic waves or particle radiation. Use according to claim 42, wherein the electromagnetic Waves or particle radiation hard X-rays with an energy of more than 12.4 keV, preferably more than 15 keV.