EP3911619A1 - Procédé de production ou de modification d'objets contenant du carbure de silicium - Google Patents

Procédé de production ou de modification d'objets contenant du carbure de silicium

Info

Publication number
EP3911619A1
EP3911619A1 EP20700189.2A EP20700189A EP3911619A1 EP 3911619 A1 EP3911619 A1 EP 3911619A1 EP 20700189 A EP20700189 A EP 20700189A EP 3911619 A1 EP3911619 A1 EP 3911619A1
Authority
EP
European Patent Office
Prior art keywords
silicon carbide
laser
additive manufacturing
precursor
silicon
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP20700189.2A
Other languages
German (de)
English (en)
Inventor
Siegmund Greulich-Weber
Rüdiger SCHLEICHER-TAPPESER
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
PSC Technologies GmbH
Original Assignee
PSC Technologies GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by PSC Technologies GmbH filed Critical PSC Technologies GmbH
Publication of EP3911619A1 publication Critical patent/EP3911619A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00—Producing shaped prefabricated articles from the material
    • B28B1/001—Rapid manufacturing of 3D objects by additive depositing, agglomerating or laminating of material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
    • B29C64/10—Processes of additive manufacturing
    • B29C64/188—Processes of additive manufacturing involving additional operations performed on the added layers, e.g. smoothing, grinding or thickness control
    • B29C64/194—Processes of additive manufacturing involving additional operations performed on the added layers, e.g. smoothing, grinding or thickness control during lay-up
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
    • B29C64/30—Auxiliary operations or equipment
    • B29C64/364—Conditioning of environment
    • B29C64/371—Conditioning of environment using an environment other than air, e.g. inert gas
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y30/00—Apparatus for additive manufacturing; Details thereof or accessories therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
    • B33Y40/20—Post-treatment, e.g. curing, coating or polishing
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/956—Silicon carbide
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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    • C04B41/4505—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application
    • C04B41/455—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application the coating or impregnating process including a chemical conversion or reaction
    • C04B41/4558—Coating or impregnating involving the chemical conversion of an already applied layer, e.g. obtaining an oxide layer by oxidising an applied metal layer
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    • C04B41/53—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone involving the removal of at least part of the materials of the treated article, e.g. etching, drying of hardened concrete
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    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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    • H01L21/0445—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising crystalline silicon carbide
    • H01L21/0455—Making n or p doped regions or layers, e.g. using diffusion
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    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
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    • C04B2111/00034—Physico-chemical characteristics of the mixtures
    • C04B2111/00181—Mixtures specially adapted for three-dimensional printing (3DP), stereo-lithography or prototyping
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Definitions

  • the present invention relates to the technical fields of additive manufacturing and surface processing.
  • the present invention relates to a method for producing or modifying objects containing silicon carbide and to the objects obtainable with the method.
  • Another object of the present invention is an apparatus for performing the method.
  • Additive manufacturing processes are increasingly used for the production of objects in small series or individual pieces made of plastics or metallic materials. Additive manufacturing enables objects to be manufactured from a large number of organic and inorganic materials both quickly and in a detailed and cost-effective manner.
  • Silicon carbide is an interesting material due to its mechanical and electrical properties for both mechanical engineering and semiconductor technology.
  • Silicon carbide with the chemical formula SiC can be used in a variety of ways in electrical engineering and for the production of ceramic materials. Due to its great hardness and high melting point, silicon carbide is also called carborundum and is used as an abrasive or as an insulator in high-temperature reactors. In addition, silicon carbide combines with a number of elements and compounds alloys or alloy-like compounds that have a variety of advantageous material properties, such as high hardness, high resistance, low weight and low oxidation sensitivity even at high temperatures .
  • Objects made of silicon carbide-containing materials are usually produced using sintering processes, the objects made of silicon carbide obtained in this way having a relatively high porosity and being unsuitable for many applications. Even a detailed and high-resolution display of small components or objects based on materials containing silicon carbide is difficult to achieve in this way.
  • Objects made of materials containing silicon carbide are not accessible from silicon carbide powders as part of additive manufacturing, since silicon carbide does not melt under normal pressure, but sublimes at temperatures of approx. 2,700 ° C.
  • the procedure is often such that the organic polymer is presented in the form of the object to be manufactured by means of additive manufacturing and the body made of organic polymer is then pyrolyzed, so that a carbon skeleton remains, which contains silicon infiltrated and finally converted to silicon carbide at high temperatures.
  • This production method for objects containing silicon carbide is very complex and time-consuming and therefore generally not very efficient.
  • Subtractive manufacturing processes are of particular importance both for surface technology and processing and in particular for the shaping of objects.
  • Subtractive manufacturing processes are generally understood to mean manufacturing processes in which material is removed from the surface of an object.
  • Subtractive manufacturing processes are usually classic machining processes, such as grinding, boring or milling.
  • Subtractive processes are used to process a variety of materials, for example to obtain the desired intermediate or end products from molded articles or to impart desired surface contours and properties to an object.
  • a further object of the present invention is to be seen in providing a method which enables localization with simple means limits to change the chemical properties of silicon carbide-containing materials, especially silicon carbide-containing surfaces.
  • the subject of the present invention according to a first aspect of the present invention is thus a method for producing and / or modifying objects containing silicon carbide according to claim 1; a further, advantageous embodiment of this aspect of the invention is the subject of the relevant subclaims.
  • Another object of the present invention in accordance with a second aspect of the present invention are the silicon carbide-containing objects obtainable by the method according to the invention.
  • Another object of the present invention according to a third aspect of the present invention is an apparatus for performing the method according to the invention according to claim 20; a further, advantageous embodiment of this aspect of the invention is the subject of the related subclaim.
  • the subject of the present invention - according to a first aspect of the present invention - is thus a method for producing and / or modifying objects containing silicon carbide, wherein
  • a surface of the at least partially produced silicon carbide-containing object is processed by ablation or by chemical modification of the surface by irradiating, in particular heating, the surface of the object in a location-selective and locally limited manner by means of at least one laser beam .
  • the method according to the invention makes it possible, in particular, to process the surfaces of objects made of materials containing silicon carbide, which, for example due to the complex geometry of the object or component produced, for machining with tools after completion of the silicon carbide, even when a large number of additive manufacturing processes have been carried out Object are no longer available.
  • a method for the ablation and / or chemical modification of surfaces of objects containing silicon carbide is combined with an additive manufacturing method, which likewise uses a laser to carry out the additive manufacturing.
  • the same devices can thus be used both for additive manufacturing and for surface processing within the scope of the present invention.
  • the surface of the silicon carbide-containing material is heated for the surface treatment, ie the surface treatment takes place thermally.
  • the ablation is carried out, for example, with excimer lasers, which emit ultrashort light pulses in the UV range, the ablation is carried out by a Coulomb explosion - as explained below - and another laser system must be used for additive manufacturing.
  • the additive manufacturing is selected from powder bed processes, in particular selective synthetic crystallization, processes based on laser cladding or processes based on inkjet printing.
  • selective synthetic crystallization an object is not created from the melt, but from the gas phase.
  • the construction and implementation of selective synthetic crystallization corresponds to selective laser melting, i.e. for the selective synthetic crystallization the same devices can be used under very similar conditions as for the selective laser melting.
  • the laser radiation allows the energy required for converting the starting materials into the gas phase to be introduced into a preferably pulverulent starting material, in particular into a precursor granulate.
  • the laser beam usually decomposes the precursor materials into gaseous products, which then recombine directly into the desired silicon carbide-containing materials and are obtained in crystalline form.
  • the surfaces of silicon carbide-containing materials and objects can be processed simply and easily by means of laser radiation, in particular by means of pulsed laser radiation, preferably using a pulse laser.
  • either diffusion processes can be generated in the surface of the silicon carbide-containing material, so that surfaces enriched with carbon or silicon, for example - surfaces can be obtained, or the material is removed by ablation, in particular by sublimation, as a result of which the surface of the object containing silicon carbide can be structured and a geometric shape of objects made of material containing silicon carbide is also possible.
  • the ultrashort laser pulse usually creates an electron-deficient zone in a small region of just a few nanometers or micrometers on the surface of the silicon carbide-containing material, so that a large number of positively charged ions are generated, which repel each other.
  • the repelling electrical forces remove particles in the nanometer range from the surface of the silicon carbide-containing material.
  • the pulse duration or length is usually in the range from 10 fs to 10 ps and the laser intensity in the range from 10 10 to 10 13 W / cm 2 . If the method is only to be used to process the surfaces using ablation, then lasers with pulse lengths in the femto or picosecond range are preferably used. An excimer laser with radiation in the UV range is particularly preferably used for this type of surface treatment.
  • the silicon carbide-containing material is only briefly and selectively exposed to the energy.
  • only one area which corresponds approximately to the width or area of the laser beam, is irradiated and processed with the laser energy by the laser radiation.
  • the depth of penetration into the silicon carbide-containing material is also only a few nanometers or micrometers. In this way, a very location-selective and locally limited processing of the surface is possible, i.e. For example, nano- or microstructures with a depth of only a few nanometers or micrometers can be produced on the surface of the silicon carbide-containing material.
  • location-selective is to be understood to mean that the laser beam or the laser beams can be directed at a defined and fixed position of the silicon carbide-containing material or a substrate.
  • locally limited preferably means that not the entire surface of the silicon carbide-containing material is affected, but rather only a sharply defined area.
  • locally limited within the scope of the present invention is understood to mean an area on the surface of the silicon carbide-containing material which corresponds to the area which is swept by the laser beam.
  • the irradiated or heated area of the silicon carbide-containing material preferably corresponds to the area which is swept by the laser beam, ie the effects of the laser beams are limited to the directly irradiated material and if possible there is little or no long-range effect.
  • an object is to be understood on the one hand to mean a three-dimensional structure, in particular a component, or also a coating, ie a layer that is only a few micrometers or millimeters thick.
  • An object containing silicon carbide is preferably to be understood as an object which contains and / or consists of material containing silicon carbide, preferably consists of material containing silicon carbide.
  • a surface of a silicon carbide-containing object means the interface of the silicon carbide-containing object, for example with the surrounding atmosphere or with other components.
  • a silicon carbide-containing material is understood to mean a material which contains or consists of compounds containing silicon carbide.
  • a compound containing silicon carbide is to be understood as a binary, ternary or quaternary inorganic compound which contains the empirical formula silicon and carbon.
  • a compound containing silicon carbide does not contain any molecularly bound carbon, such as, for example, carbon monoxide or carbon dioxide; rather, the carbon is in a solid structure.
  • the silicon carbide-containing material is usually selected from silicon carbide, doped silicon carbide, non-stoichiometric silicon carbide, doped non-stoichiometric silicon carbide and silicon carbide alloys. A large number of different silicon carbide-containing materials, in particular different silicon carbide compounds, can thus be processed with the method according to the invention.
  • a non-stoichiometric silicon carbide is understood to mean a silicon carbide which contains carbon and silicon contains not in a molar ratio of 1: 1, but in different ratios.
  • a non-stoichiometric silicon carbide usually has a molar excess of silicon.
  • silicon carbide alloys are to be understood as meaning compounds of silicon carbide with metals, such as, for example, titanium or also other compounds, such as zirconium carbide or boron nitride, which contain silicon carbide in different and widely fluctuating proportions. Silicon carbide alloys often form high-performance ceramics, which are characterized by particular hardness and temperature resistance.
  • the non-stoichiometric silicon carbide is usually a silicon carbide of the general formula (I)
  • SiC-i- x (I) with x 0.05 to 0.8, in particular 0.07 to 0.5, preferably 0.09 to 0.4, preferred
  • Such silicon-rich silicon carbides have a particularly high mechanical strength and are suitable for a large number of applications as ceramics.
  • the silicon carbide-containing compound is a doped silicon carbide
  • the silicon carbide is usually doped with an element selected from the group consisting of nitrogen, phosphorus, arsenic, antimony, boron, aluminum, gallium, indium and mixtures thereof.
  • the silicon carbide is preferably doped with elements of the 13th and 15th group of the periodic table of the elements, as a result of which in particular the electrical properties of the silicon carbide can be manipulated and adjusted in a targeted manner. Doped silicon carbides of this type are particularly suitable for applications in semiconductor technology.
  • the doped silicon carbide can be a stoichiometric silicon carbide or a non-stoichiometric silicon carbide, the doping of stoichiometric silicon carbides being preferred since these are increasingly being used in semiconductor technology. If a doped silicon carbide is used in the context of the present invention, it has proven useful if the doped silicon carbide contains the doping element in amounts of 0.000001 to 0.0005% by weight, in particular 0.000001 to 0.0001% by weight. %, preferably 0.000005 to 0.0001% by weight, preferably 0.000005 to 0.00005% by weight, based on the doped silicon carbide. For the targeted adjustment of the electrical properties of the silicon carbide, extremely small amounts of doping elements are therefore sufficient. The quantities of the doping elements mentioned above apply to both stoichiometric and non-stoichiometric silicon carbides.
  • the silicon carbide-containing compound used in the context of the present invention is a silicon carbide alloy
  • the silicon carbide alloy is usually selected from MAX phases, alloys of silicon carbide with elements, in particular metals, and alloys of silicon carbide with metal carbides and / or metal nitrides.
  • Such silicon carbide alloys contain silicon carbide in varying and strongly fluctuating proportions.
  • silicon carbide is the main constituent of the alloys.
  • the silicon carbide alloy usually has the silicon carbide in amounts of 10 to 95% by weight, in particular 15 to 90% by weight, preferably 20 to 80% by weight, based on the silicon carbide alloy.
  • M stands for an early transition metal from the third to sixth group of the Periodic Table of the Elements, while A stands for an element of the 13th to 16th Group of the Periodic Table of the Elements.
  • X is either carbon or nitrogen.
  • MAX phases are of interest, the sum formula of which contains silicon carbide (SiC), ie silicon and carbon.
  • MAX phases have unusual combinations of chemical, physical, electrical and mechanical properties, since they show both metallic and ceramic behavior depending on the conditions. This includes, for example, high electrical and thermal conductivity, high load Ability to thermal shock, very high hardness and low thermal expansion coefficient.
  • the silicon carbide alloy is a MAX phase
  • the MAX phase is selected from TUSiC 3 and T SiC.
  • the aforementioned MAX phases in particular are highly resistant to chemicals and oxidation at high temperatures.
  • the silicon carbide-containing compound is an alloy of the silicon carbide, it has proven itself in the case that the alloy is an alloy of silicon carbide with metals, if the alloy is selected from alloys of silicon carbide with metals from the group of Al, Ti, V, Cr, Mn, Co, Ni, Zn, Zr and their mixtures.
  • the alloy of silicon carbide is selected from alloys of silicon carbide with metal carbides and / or nitrides, it has proven useful if the alloys of silicon carbide with metal carbides and / or nitrides is selected from the group of boron carbides, in particular B 4 C, chromium carbides, in particular Cr 2 C 3 , titanium carbides, in particular TiC, molybdenum carbides, in particular M0 2 C, niobium carbides, in particular NbC, tantalum carbides, in particular TaC, vanadium carbides, in particular VC, zirconium carbides, in particular ZrC, tungsten carbides, in particular WC, boron nitride, in particular BN, and their mixtures.
  • boron carbides in particular B 4 C
  • chromium carbides in particular Cr 2 C 3
  • titanium carbides in particular TiC
  • molybdenum carbides in particular M0 2 C
  • niobium carbides in particular Nb
  • additive manufacturing is a manufacturing process which is carried out with the aid of laser radiation.
  • the use of additive manufacturing processes which include the production of silicon carbide-containing materials by using laser energy or beams, has the advantage that ideally the same laser that is used for additive manufacturing also for ablation or chemical modification of the surface of the silicon carbide-containing object can be used.
  • the same apparatus structure can thus be used both for carrying out additive manufacturing and for surface processing, which significantly simplifies the implementation of the method within the scope of the invention and makes the apparatus construction very cost-effective.
  • the surface treatment in particular the ablation
  • the device for carrying out the method has at least two different lasers or the additive manufacturing and surface treatment are carried out with different lasers.
  • the usual procedure is to deposit a layer of silicon carbide-containing material on a substrate in a location-selective manner, so that a layer or layer from which the object is built is obtained.
  • a further layer of silicon carbide-containing material is then deposited in a location-selective manner on the previously obtained layer, so that a further layer of the object containing silicon carbide-containing material or consisting of silicon carbide-containing material is obtained.
  • step (b) i.e. to be carried out in the surface processing step following the additive manufacturing or also during the additive manufacturing, for example after building up one or more layers of the object containing silicon carbide.
  • the silicon carbide-containing material is obtained by decomposing precursor materials and is deposited on a surface, in particular a substrate.
  • gaseous, liquid or solid precursors containing a carbon source and a silicon source are irradiated, in particular decomposed, by means of a laser beam, and the silicon carbide-containing material is deposited on a surface, in particular a substrate.
  • additive manufacturing can be selected from all suitable methods. However, particularly good results are obtained when additive manufacturing is selected from selective synthetic crystallization, printing processes with subsequent laser irradiation and laser cladding, and processes based on these processes.
  • the additive manufacturing is selected from powder bed processes, in particular the Selective synthetic crystallization, processes based on laser cladding or processes based on inkjet printing.
  • the selective synthetic crystallization is described for example in DE 10 2017 1 10 362 A1.
  • powdery precursor materials are converted to silicon carbide-containing materials by irradiation with a laser beam.
  • a suitable inkjet process is described in DE 10 2017 110 361 A1.
  • liquid precursor materials are applied to a substrate surface by means of an inkjet printing process and then converted to the corresponding silicon carbide-containing materials by the action of laser radiation.
  • a particle beam of solid, liquid or gaseous particles is directed onto a substrate surface and is irradiated by means of a laser beam when or before it hits the substrate surface, so that the precursor compounds are decomposed and selectively converted to silicon carbide.
  • the procedure is usually such that a so-called digital twin of the object is created before the silicon carbide-containing object is produced.
  • the creation of a digital image of the object to be produced enables, in particular, a digital model of the object to be produced with almost any resolution and accuracy, with the aid of which the production can subsequently be carried out, in particular by means of additive and subtractive production or by means of additive production and chemical modification .
  • the digital image is created by means of geometric modeling, in particular by means of CAD.
  • CAD Computer Aided Design
  • CAD Computer Aided Design
  • the arrangement and size of the individual layers can also be calculated, which are necessary for producing an object, in particular a three-dimensional object or a component.
  • the object containing silicon carbide is produced by comparison with the digital image.
  • the combination of additive and subtractive manufacturing possibly in combination with a chemical modification of the surface, creates an object that is as accurate and high-contrast as possible, high-resolution silicon carbide-containing object.
  • the digital image deviates from the specifics in the manufacturing process, such as thermal conditions, by a predetermined amount from the object to be produced.
  • fluctuations in size or distortion caused by heating and cooling of the object containing silicon carbide or the partially finished object containing silicon carbide must always be taken into account. This applies in particular to objects made of silicon carbide or doped silicon carbide containing silicon carbide and to objects made of silicon carbide alloys to a much lesser extent, since these have only a low thermal expansion.
  • the method according to the invention also allows, for example, a partial modification of the silicon carbide-containing object of the surface of individual layers applied during additive manufacturing, the chemical properties and subsequently also the electrical properties of silicon carbide-containing materials in the interior of an object which contains silicon carbide-containing materials or therefrom consists of hiring specifically. In this way, for example, it is possible to specifically produce conductor tracks for conducting electrical currents inside an object from material containing silicon carbide.
  • the object containing silicon carbide is measured during and / or after the additive manufacturing.
  • the additive manufacturing is carried out by means of a laser and the laser which is used for the additive manufacturing is also used for the measurement of the manufactured object at the same time. This can be done, for example, using an interferometer.
  • Particularly good results are obtained in this connection if the object is measured during and / or after additive manufacturing and the surface of the object is processed after comparison with the digital image, so that the object and the digital image match or to a predetermined extent differ from each other.
  • the surface of the object is processed during or after additive manufacturing. This means that even the object that has not yet been completely manufactured can already be irradiated with laser radiation and processed by means of ablation or chemical modification before the additive manufacturing has been completed.
  • the surface of the silicon carbide-containing material is heated. If the surface of the silicon carbide-containing object is heated by means of the laser beam, it has proven useful if the surface of the silicon carbide-containing object is at temperatures in the range from 500 to 3,500 ° C., in particular 600 to 3,200 ° C., preferably 700 to 3,000 ° C. C, is heated. At temperatures in the aforementioned range, either chemical modifications of the silicon carbide-containing material of the object or structural processing by means of ablation can be carried out.
  • the surface of the silicon carbide-containing object is processed by means of ablation. This means that the surface of the silicon carbide-containing object by means of subtractive manufacturing, i.e. under material removal.
  • the surface of the object containing silicon carbide is structured and / or smoothed, in particular microstructured and / or smoothed, or that the object containing silicon carbide is geometrically processed by means of ablation.
  • Structuring the surface of the silicon carbide-containing object is to be understood in particular to mean that defined and defined structures, preferably in the nanometer or micrometer range, ie so-called microstructures, are produced on the surface of the silicon carbide-containing material in order, for example, to adjust the surface roughness of the silicon carbide-containing material or also to provide structures for micromechanical systems. Equally, however, it is also possible for the surface to be smoothed, for example after the additive manufacturing.
  • the layer-like structure of the manufactured object, which is caused by the additive manufacturing, can often still be recognized, in particular at the interfaces of the object.
  • surface treatment in particular smoothing
  • the object containing silicon carbide is at least partially subjected to shaping by ablation, in particular by the action of laser beams. Material can be removed in the range of micrometers to millimeters or even to the centimeter by repeated or continuous exposure to the laser beam. The ablation is therefore suitable, for example, for removing support structures which are used in additive manufacturing.
  • elevations can be flattened, for example, because the elevations heat up more quickly and material is removed there before depressions occur stay cooler due to better heat conduction, deepen.
  • Ablation by means of laser radiation also opens up new possibilities for microstructured surfaces containing silicon carbide due to the possibility of reproducibly and with high precision in the nanometer or micrometer range, in conjunction with the high strength of silicon carbide and materials containing silicon carbide.
  • the roughness of the surface of the silicon carbide-containing object in a targeted manner for mechanical applications.
  • surfaces of objects containing silicon carbide can be specifically structured for micromechanical applications.
  • the electrical and physical properties of electrodes and membranes can be influenced by targeted structuring, in particular the electrochemical properties can also be specifically adjusted.
  • the structuring of the surfaces of objects containing silicon carbide can also be used in the field of semiconductor technology. se structuring of semiconductor layers with different functions. Equally, it is also possible to obtain complex three-dimensional structures by successively applying a plurality of two-dimensionally structured materials, first of all producing a first layer, in particular by means of additive manufacturing, and then structuring by means of ablation under the influence of laser radiation, whereupon a second layer by means of additive manufacturing is applied and also structured.
  • the surface of the object to be processed containing silicon carbide is usually precisely measured.
  • either laser processing or scanning passes of the surface can be carried out alternately, or a real-time measurement of the surface of the object containing silicon carbide can be carried out.
  • a real-time measurement of the currently processed part of the surface is preferably carried out, in particular a measurement of the processed surface segment is possible by measuring the reflected laser beam using an interferometer.
  • a comparison with a digital image, in particular a digital twin, then enables real-time control of both the irradiation location of the laser radiation and the laser power in order to achieve the desired material removal in a targeted manner.
  • the surface of the object containing silicon carbide is processed by ablation, it has proven useful if the surface of the object containing silicon carbide is heated to temperatures above 2,200 ° C., in particular above 2,500 ° C., preferably above
  • 2,700 ° C, preferably above 2,900 ° C, is heated.
  • sublimation of silicon carbide-containing materials is usually possible.
  • the surface of the object containing silicon carbide is heated to temperatures in the range from 2,200 to 3,500 ° C., in particular from 2,500 to 3,300 ° C., preferably from 2,700 to 3,200 ° C., preferably from 2,900 to 3,000 ° C. becomes.
  • ablation i.e. material removal of the silicon carbide-containing material is also possible without significant heating of the silicon carbide-containing material by using pulse lasers with pulse lengths in the range of 10 ps or less.
  • the pulse lasers used for this case usually have pulse lengths in the range from 1 fs to 10 ps, in particular 10 fs to 10 ps, preferably 10 fs to 2 ps, preferably 10 fs to 100 fs.
  • the laser radiation can also be used to achieve a chemical modification of the surface of the object containing silicon carbide.
  • the chemical modification of the surface is usually selected from the group consisting of an accumulation of silicon on the surface of the silicon carbide-containing material, an accumulation of carbon on the surface of the silicon carbide-containing material, formation of graphene and / or graphite on the surface of the silicon carbide-containing material, the formation of silicon dioxide on the surface of the silicon carbide-containing material and their combinations.
  • the temperatures for the chemical modification of the surface of the silicon carbide-containing material are usually not chosen to be as high as for an ablation of the silicon carbide-containing object.
  • the increase in temperature triggers diffusion processes in the immediate vicinity of the surface, which lead, for example, to an accumulation of silicon or carbon and finally to the formation of carbon, in particular the formation of graphene and / or graphite, on the surface of the object containing silicon carbide.
  • the formation of thin silicon oxide layers is also possible if the surface is heated in the presence of small amounts of oxygen.
  • the chemical modification of the surface of the silicon carbide-containing object makes it possible to change the properties, in particular the electrical properties, of the silicon carbide-containing material in a targeted, location-selective and locally limited manner.
  • the surface of the silicon carbide-containing material is usually heated to temperatures above 500 ° C., in particular above 600 ° C., preferably above 700 ° C. , preferably above 750 ° C, heated.
  • the surface of the silicon carbide-containing object is heated to temperatures in the range from 500 to 2,000 ° C., in particular 600 to 1,800 ° C., preferably 700 to 1,600 ° C., preferably 750 to 1,500 ° C.
  • the chemical modification on the surface of the silicon carbide-containing object usually takes place only to a depth of a few micrometers or nanometers, in particular less than 1 pm, preferably less than 100 nm.
  • silicon diffuses to the surface of the silicon carbide-containing object Object on and from 800 ° C there is a silicon desorption from the surface of the objects containing silicon carbide.
  • silicon is rapidly desorbed from the silicon carbide-containing surface and the formation of graphene begins.
  • the formation of graphene follows successively, in that layer of graphene is formed layer by layer, whereby, before a new layer of graphene is formed, a layer of silicon carbide-containing material first forms a carbon-rich silicon carbide, which is finally converted into graphene by further desorption of silicon.
  • the formation of graphene proceeds from the surface of the object into ever deeper layers of the silicon carbide-containing object. If the surface of the silicon carbide-containing object is heated in the presence of oxygen, silicon dioxide forms on the surface of the silicon carbide-containing material.
  • the silicon dioxide layer is very thin and has only a few lattice constants and is limited in its growth.
  • the Silicon dioxide surface layer serves as a protective layer for the underlying silicon carbide-containing material and prevents decomposition of the silicon carbide.
  • the process in particular process step (b), is preferably carried out in a vacuum, preferably in an ultra-high vacuum.
  • the chemical modification of the surface of the silicon carbide-containing object makes the surface of the silicon carbide-containing material for doping, in particular for a treatment with doping reagents.
  • the defective structures or defects in the structure of the silicon carbide-containing material of the silicon carbide-containing object can be generated, into which the corresponding doping elements, in particular elements of the 3rd and 5th main groups of the periodic table of the Elements that can be introduced.
  • the doping elements can be applied to the surface of the silicon carbide-containing object, for example, either via the gas phase or by treating the surface of the silicon carbide-containing material, in particular the activated surface, with liquids, in particular with solutions or dispersion, which contain compounds of the doping elements.
  • the conversion to the correspondingly doped silicon carbide-containing materials can take place either by annealing the silicon carbide-containing object at elevated temperatures, in particular at temperatures above 1,300 ° C., or by irradiation with a laser beam.
  • the solution or dispersion of the doping reagent usually has an amount of from 0.000001 to 0.5% by weight, preferably 0.000005 to 1% by weight, preferably 0.000001 to 0.1% by weight, based on the solution of the dispersion.
  • the chemical nature of the doping reagent it usually contains at least one doping element.
  • the doping element is preferably selected from elements of the third and fifth main groups of the periodic table.
  • the doping reagent is preferably selected from compounds of an element of the third or fifth main group of the Periodic Table of the Elements, which is soluble or finely dispersible in a solvent or dispersant.
  • the doping reagent is usually selected from nitric acid, ammonium chloride, melamine, phosphoric acid, phosphonic acids, boric acid, borates, boron chloride, indium chloride and mixtures thereof.
  • the solution may contain nitric acid, ammonium chloride or melanin. If doping with phosphorus is provided, phosphoric acid or phosphates or phosphonic acids can be used, for example. In addition, nitrogen doping is also possible by carrying out the method according to the invention in a nitrogen atmosphere.
  • boric acids borates or boron salts such as boron trichloride, for example, are used.
  • indium is doped
  • water-soluble indium salts such as indium chloride, are usually used as the doping reagent.
  • the process is usually not carried out in a standard atmosphere.
  • the process is carried out in an atmosphere containing at most 5% by volume of oxygen or in vacuo.
  • the atmosphere in which the process is carried out does not exceed 3% by volume, in particular does not exceed 2% by volume, preferably does not exceed 1% by volume, preferably does not exceed 0.5% by volume .-% contains oxygen.
  • the atmosphere in which the process is carried out contains 0 to 5% by volume of oxygen, in particular 0.01 to 3% by volume of oxygen, preferably 0.05 to 2% by volume of oxygen, preferably contains 0.08 to 1% by volume of oxygen, particularly preferably 0.1 to 0.5% by volume of oxygen.
  • the process according to the invention is preferably carried out in an oxygen-free atmosphere or in a vacuum, in particular in a high vacuum.
  • Small amounts of oxygen are only used in the process or process atmosphere when a targeted oxidation of the silicon to silicon dioxide and an oxidation of the carbon to carbon dioxide are to take place in the uppermost layer of the material containing silicon carbide or the object containing silicon carbide.
  • an inert gas is to be understood as a gas which, under process conditions, does not react with the silicon carbide-containing material and is also not incorporated therein.
  • a particularly preferred inert gas in the context of the present invention is argon.
  • doping of silicon carbide-containing materials can be achieved in regions if the atmosphere in which the method according to the invention is carried out contains doping elements or doping reagents, such as elemental nitrogen.
  • doping elements or doping reagents such as elemental nitrogen.
  • volatile organyls or hydrides of compounds of the 3rd and 5th main group of the Periodic Table of the Elements which in particular pass into the gas phase under reduced pressure and can be used as doping reagents.
  • the laser beams for surface processing are generated by means of a pulse laser. If the laser beams are generated by means of a pulse laser which has a pulse length of more than 10 ps, in particular in the nanosecond range, the surface of the object containing silicon carbide is primarily heated. Through targeted and locally limited warming In particular, the chemical modification or the ablation of the material containing silicon carbide can be controlled in a targeted manner on the surface of the object containing silicon carbide. In addition, as already mentioned above, it is also possible within the scope of the present invention for the laser beams to be generated by an ultrashort pulse laser.
  • an ultrashort pulse laser with pulse lengths of 1 fs to 10 ps, in particular 10 fs to 2 ps, preferably 10 fs to 100 fs, can be used for the ablation.
  • the use of such ultrashort pulse lasers, in particular with radiation in the UV range, enables an almost heat-free ablation of the surface of materials or objects containing silicon carbide.
  • the laser radiation in particular for carrying out additive manufacturing and / or for heating the surface of the silicon carbide-containing object, has a wavelength in the visible range or in the IR range. If the surface of the object containing silicon cabride is thermally processed, laser radiation in the visible or IR range can often be used, and in particular the same laser can be used for additive manufacturing and surface processing.
  • the laser radiation in particular for performing the ablation, has a wavelength in the UV range.
  • This embodiment of the present invention is used in particular when using excimer lasers, different lasers being used here preferably for additive manufacturing and surface processing of the object containing silicon carbide.
  • the process progress in particular the ablation, is monitored, in particular continuously monitored.
  • silicon carbide-containing materials in particular in the form of layers
  • the layer of silicon carbide-containing material can completely or only partially cover the substrate surface.
  • both targeted coating of objects can be carried out and three-dimensional objects can be produced from materials containing silicon carbide.
  • the additive manufacturing is preferably carried out in the form of selective synthetic crystallization, printing processes with subsequent laser radiation, laser deposition welding or processes based on these.
  • the method based on laser cladding is usually a method for applying silicon carbide-containing materials to a substrate surface, whereby a gaseous, liquid or powdered precursor material containing a silicon source and a carbon source is gasified and / or decomposed by the action of laser radiation and at least a part of it Decomposition products are deposited selectively on the substrate surface as silicon carbide-containing material.
  • This additive process allows the creation of high-resolution and detailed three-dimensional structures, ie the course of contours, such as corners or edges, is highly precise and in particular free of burrs.
  • this additive method allows a very fast and inexpensive production of three-dimensional objects or coatings containing silicon carbide and in particular does not require the use of pressure in order to provide compact, non-porous materials.
  • coatings made of silicon carbide-containing materials can be applied to a substrate surface and three-dimensional objects made of silicon carbide-containing materials.
  • the precursor material in particular the powdered precursor material
  • the precursor material is moved in the direction of the substrate in a finely divided and directed form, in particular in the form of at least one particle beam, and before or gasified and decomposed when it hits the substrate by the action of energy, in particular laser radiation, or that the gaseous decomposition products are moved in the direction of the substrate, in particular in the form of a particle beam.
  • a particle beam is to be understood as a directed flow of particles or particles with a cross section that preferably remains constant, which preferably moves linearly.
  • the precursor materials or the decomposition products can be moved in one or more particle beams in the direction of the substrate surface and, for example, at a focal point, e.g. the light beam of a laser, or on the substrate surface.
  • the particle beam or the particle beams is or are preferably directed onto the substrate surface.
  • the starting compounds to be moved in a finely divided form, preferably in the form of a finely divided powder, in particular a powder jet, in the direction of the substrate surface and before, in particular immediately before, or when it strikes the substrate surface through the action of energy, in particular through the action of a serstrahls, gasified and decomposed.
  • the decomposition products are generated in the immediate vicinity of the surface to which they are applied and can be deposited on the cooler substrate surface in a preferably single-crystalline form.
  • the decomposition products it is also possible for the decomposition products to be moved, for example, through a nozzle in the direction of the substrate surface and to be applied thereon, the decomposition products being deposited at least in part on the substrate surface as the desired silicon carbide-containing material.
  • the decomposition products there is always the risk that larger agglomerates will form in the gas phase and that a less dense and homogeneous surface will be obtained.
  • the precursor material in particular the powdered precursor material, or the gaseous decomposition products is or are moved in the direction of the substrate by means of at least one nozzle.
  • a nozzle By using a nozzle, it is in particular possible to obtain a sharply defined particle beam, preferably from gaseous particles or from powder particles, which are applied to the substrate surface in a location-selective manner.
  • the nozzle is particularly preferably a powder nozzle or a gas nozzle.
  • the nozzle can either be arranged coaxially to, for example, a laser beam or laterally.
  • the laser beam and nozzle are generally located in a processing head or an assembly, the laser beam being directed almost perpendicularly to the substrate surface and the particle beam intersecting it or several particle beams intersecting the axis of the laser beam at a focal point.
  • the laser beam is usually also arranged and movable perpendicular to the substrate surface, a particle stream being injected laterally into the axis of the laser beam.
  • the use of powdered precursor materials is preferred, although gaseous or liquid precursor materials can also be used.
  • the powdered precursor material is moved in the form of a powder jet in the direction of the substrate or that the liquid precursor material is moved in atomized form or as a liquid jet in the direction of the substrate, preferably but always in the form of a particle beam.
  • the gaseous precursor material it is also possible for the gaseous precursor material to be moved in the direction of the substrate in the form of a gas stream.
  • the gaseous decomposition products it is also possible for the gaseous decomposition products to be moved in the direction of the substrate in the form of a gas jet.
  • the additive manufacturing is a laser cladding or a method based on laser cladding, in which the precursor materials are gasified and / or decomposed before or until contact with the substrate surface.
  • the precursor material in particular the powdered precursor material
  • the precursor material is gasified and decomposed in the vicinity of the substrate surface by means of laser radiation, in particular in the immediate vicinity of the substrate surface.
  • the substrate is heated only very slightly by the energy introduced, in particular by the laser beam, so that, on the one hand, the silicon carbide-containing material can be applied as stress-free as possible.
  • a silicon source or a carbon source means compounds which can release silicon or carbon under process conditions in such a way that compounds containing silicon carbide are formed.
  • silicon and carbon do not have to be released in elemental form, but it is sufficient if they react to silicon carbide-containing compounds under process conditions.
  • a substrate is to be understood as the material to which the - in particular gaseous - decomposition products of the precursor material are applied.
  • a substrate in the context of the present invention is a three-dimensional or even an almost two-dimensional structure with a surface on which the decomposition products of the precursor material are deposited as silicon carbide-containing material.
  • the substrate surface can be flat or contoured, in particular three-dimensionally structured.
  • the substrate can have almost any three-dimensional shape.
  • the substrate can thus be a carrier material on which silicon carbide-containing material is deposited in layers.
  • the term substrate in particular also includes carrier materials which are partially coated with one or more layers of materials containing silicon carbide.
  • a substrate can also be a three-dimensional object which is joined to a second substrate, in particular a further three-dimensional object, by deposited silicon carbide-containing material.
  • the precursor material is first applied to a substrate and then decomposed in a location-selective manner.
  • liquid precursors are applied to a substrate surface, however in a location-selective manner and decomposed.
  • the substrate to which the precursor material or its decomposition products are applied this can be selected from a large number of suitable materials.
  • the substrate is possible for the substrate to be selected from crystalline and amorphous substrates.
  • the substrate is an amorphous substrate.
  • the material is selected from carbon, in particular graphite, and ceramic materials, in particular silicon carbide, silicon dioxide, aluminum oxide and metals and their mixtures.
  • the substrate often has several materials, in particular a carrier material and the three-dimensional object made of silicon carbide-containing material that is at least partially built thereon.
  • the precursor material used for additive manufacturing is preferably selected from gaseous, liquid or powdered precursor materials.
  • the liquid precursor material can a homogeneous solution or a dispersion, in particular also a solid-in-liquid dispersion.
  • a precursor material is to be understood as a chemical compound or a mixture of chemical compounds which react under process conditions to the desired product materials, in particular materials containing silicon carbide.
  • the reaction to the target compounds can take place in various ways. However, it is advantageously provided that the precursor compounds are split or decomposed under the action of energy, in particular under the action of a laser beam, and pass into the gas phase as reactive particles. Since silicon and carbon as well as optionally doping or alloying elements are immediately adjacent in the gas phase due to the special composition of the precursor, the silicon carbide or the doped silicon carbide or silicon carbide alloy, which only sublimates at 2,300 ° C., is separated. In particular, crystalline silicon carbide absorbs laser energy much less well than the precursor materials and conducts heat very well, so that the defined silicon carbide compounds are deposited in a strictly local manner. In contrast, undesired constituents of the precursor compound preferably form stable gases, such as, for example, CO2, HCl, H2O etc., and can be removed via the gas phase.
  • stable gases such as, for example, CO2, HCl, H2O etc.
  • the precursor material is a solid precursor material, in particular a precursor granulate.
  • a precursor granulate is preferably used as the precursor material for the method according to the invention.
  • the precursor material can change into the gas phase or the precursor compounds can react to the desired target compounds by means of short exposure times of energy, in particular laser radiation, individual particles of different inorganic substances with particle sizes in the mh range, their components, not having to be sublimed then diffuse to form the appropriate compounds and alloys.
  • homogeneous precursor granules preferably used or in liquid and gaseous precursors the individual building blocks, in particular elements, of the target compound containing silicon carbide are homogeneously distributed and arranged in close proximity to one another, ie less energy is required to produce the compounds containing silicon carbide.
  • This has the advantage that a multilayer structure of silicon carbide-containing material can be built up without the uppermost layer of the silicon carbide-containing material forming the substrate surface being heated to temperatures at which silicon carbide sublimes.
  • the precursor granulate is usually obtainable from a precursor solution or a precursor dispersion, in particular a precursor sol.
  • the precursor granules are thus preferably obtained in finely divided form from a liquid, in particular from a solution or dispersion.
  • a homogeneous distribution of the individual components, in particular precursor compounds can be achieved in the granulate, the stoichiometry of the silicon carbide-containing material to be produced preferably being pre-formed.
  • the precursor solution or dispersion, in particular the precursor sol can be used directly for printing processes, in particular ink jet processes.
  • the precursor granules are obtainable from a solution or dispersion, in particular a gel
  • the precursor granules are obtained by drying the precursor solutions or dispersions or the resulting gel.
  • the particle sizes of the precursor granules can vary widely depending on the respective chemical compositions, the laser energy used and the properties of the material or object to be produced.
  • the precursor granules have particle sizes in the range from 0.1 to 150 pm, in particular 0.5 to 100 pm, preferably 1 to 100 pm, preferably 7 to 70 pm, particularly preferably 20 to 40 pm.
  • the particles of the precursor granules have a D60 value in the range from 1 to 100 pm, in particular 2 to 70 pm, preferably 10 to 50 pm, preferably 21 to 35 pm.
  • the D60 value for the particle size represents the limit below which the particle size of 60% the particle of the precursor granules lies, ie 60% of the particles of the precursor granules have large particles which are smaller than the D60 value.
  • the precursor granulate has a bimodal particle size distribution. In this way, particularly precursor granules with a high bulk density are accessible.
  • the precursor material in particular the precursor granulate or a precursor sol, in particular at least in regions to temperatures in the range from 1,600 to 2,100 ° C, in particular 1,700 to 2,000 ° C, preferably 1,700 to 1,900 ° C, is heated.
  • the precursor material in particular the precursor granulate or a precursor sol, in particular at least in regions to temperatures in the range from 1,600 to 2,100 ° C, in particular 1,700 to 2,000 ° C, preferably 1,700 to 1,900 ° C.
  • additive manufacturing can also be carried out with gaseous precursor materials, in particular in processes based on laser cladding.
  • the precursor materials are decomposed by the action of energy and at least some of the decomposed precursor materials are deposited in a location-selective manner on the substrate surface as silicon carbide-containing material.
  • the silicon carbide-containing material is selected from optionally doped silicon carbide, optionally doped non-stoichiometric silicon carbide, silicon carbide alloys and mixtures thereof.
  • silicon carbide, in particular doped stoichiometric silicon carbide from precursor compounds, in particular powdery precursor compounds is known in principle and is practiced, for example, in the context of German patent application 10 2015 105 085.4.
  • precursor materials are described in more detail below. Within the scope of the present invention it can be provided, for example, that precursor materials are used which are either mixtures of liquid and / or gaseous carbon and silicon sources, ie compounds which release carbon or silicon or reactive intermediates under reaction conditions, or liquid solutions or Dispersions that have the carbon and silicon sources.
  • liquid and / or gaseous carbon sources are used as precursor materials in the context of the present invention, it can be provided that the liquid and / or gaseous carbon source is selected from alkanes, amines, alkyl halides, aldehydes, ketones, carboxylic acids, amides, carboxylic acid esters and their mixtures, in particular Cr to Cs alkanes, primary and secondary Cr to C 4 alkylamines, Cr to Cs alkyl halides, Cr to Cs aldehydes, Cr to Cs ketones, Cr to Cs carboxylic acids, Cr to Cs amides, Cr to Cs- carboxylic acid esters and their mixtures.
  • the gaseous and / or liquid carbon source is selected from Cr to Cs alkanes, in particular Cr to C 4 alkanes, and mixtures thereof.
  • the gaseous or liquid carbon source is a short-chain and thus readily volatile alkane.
  • care must be taken to ensure that the excess of carbon is so high that carbon is always oxidized to carbon monoxide or carbon dioxide and that silicon is not oxidized to silicon dioxide or silicon dioxide is immediately reduced again by carbon, since silicon dioxide would significantly disrupt the structure and function of the fibers or foams containing silicon carbide.
  • liquid and / or gaseous silicon source is selected from silanes, siloxanes and their mixtures, preferably silanes.
  • siloxanes are used as precursors, it is possible, when selecting suitable siloxanes, that the siloxane or siloxanes represent or represent both the carbon source and the silicon source and that no further precursors with the exception of any doping or alloying reagents have to be used.
  • solid, in particular powdery, precursor materials are preferably used.
  • the solid precursor materials are usually in the form of a precursor granulate containing
  • the silicon source is usually selected from silane hydrolyzates and silicas and their mixtures.
  • the silicon source i. H. the precursor of the silicon in the silicon carbide-containing compound, in particular obtained by flydrolysis of tetraalkoxysilanes, as a result of which the silicon is preferably present in the precursor granules in the form of silicic acid or silane hydrolyzates.
  • the carbon source in the precursor granules is usually selected from the group of sugars, in particular sucrose, glucose, fructose, invert sugar, maltose; Strength; Starch derivatives and organic polymers, in particular phenol-formaldehyde resin, resorcinol-formaldehyde resin, and their mixtures and / or their reaction product, in particular sugars and / or their reaction products.
  • the carbon source is particularly preferably selected from sugars and their reaction products, preferably sucrose and / or invert sugar and / or their reaction products being used. In the case of the carbon source as well, not only the actual reagent but also its reaction product can be used. If a (stoichiometric) silicon carbide is produced with the precursor granules, the composition usually contains
  • (C) optional precursors of doping elements (C) optional precursors of doping elements.
  • the precursors for the doping elements are usually contained in the precursor granules only in very small amounts, in particular in the ppm range.
  • the composition usually contains
  • the silicon source in amounts of 60 to 90% by weight, in particular 65 to 85% by weight, preferably 70 to 80% by weight, based on the composition,
  • Precursor granules which have the carbon source and the silicon source in the abovementioned quantity ranges can be used to produce non-stoichiometric silicon carbides with an excess of silicon in an outstandingly reproducible manner.
  • the composition usually contains
  • a preferably used precursor granulate can be obtained from a precursor solution or a precursor dispersion.
  • the precursor granules can be obtained by a sol-gel process or by drying a sol.
  • sol-gel processes solutions or finely divided solid-in-liquid dispersions are usually produced, which by subsequent aging and the condensation processes that occur are converted into a gel that contains larger solid particles.
  • a particularly homogeneous composition in particular a suitable precursor granulate, can be obtained, with which the desired silicon carbide-containing compounds can be obtained under the influence of energy in an additive manufacturing process when a suitable stoichiometry is selected.
  • the precursor granules are converted into reduced precursor granules by thermal treatment under reductive conditions.
  • the reductive thermal treatment usually takes place in an inert gas atmosphere, in particular the carbon source, preferably a sugar-based carbon source, with oxides or other compounds of silicon and possibly other compounds of other elements, whereby the elements are reduced and volatile oxidized carbon and hydrogen compounds, in particular Water and CO 2 arise, which are removed via the gas phase.
  • Precursor granules can be produced in particular by a sol-gel process, wherein
  • reaction product from the second process step (ii), in particular the gel is dried and optionally comminuted.
  • a method for producing a suitable precursor granulate for producing silicon carbide by means of a sol-gel method is mentioned, for example, in German patent application DE 10 2015 105 085.4.
  • a solution is to be understood as a single-phase system in which at least one substance, in particular a compound or its components, such as ions, is present in a homogeneous distribution in another substance.
  • a dispersion is to be understood as an at least two-phase system, with a first phase, namely the dispersed phase, being distributed in a second phase, the continuous phase.
  • the continuous phase is also called the dispersing medium or dispersing agent.
  • the transition from a solution to a dispersion is often fluid, particularly in the case of brines or also polymeric compounds, so that it is no longer possible to clearly differentiate between a solution and a dispersion.
  • solvent or dispersing agent in process step (a) can be selected from all suitable solvents or dispersing agents.
  • the solvent or dispersant is selected from water and organic solvents and also their mixtures, preferably their mixtures.
  • inorganic hydroxides, in particular metal hydroxides and silicas are often formed by the hydrolysis reaction of the starting compounds and subsequently condense, so that the process can be carried out either in the form of a sol-gel process or at the stage of Sols is stopped.
  • the solvent is selected from alcohols, in particular methanol, ethanol, 2-propanol, acetone, ethyl acetate and mixtures thereof.
  • the organic solvent is selected from methanol, ethanol, 2-propanol and mixtures thereof, ethanol being particularly preferred.
  • the aforementioned organic solvents are miscible with water in a wide range and are also particularly suitable for dispersing or dissolving polar inorganic substances.
  • Mixtures of water and at least one organic solvent, in particular mixtures of water and ethanol, preferably as solvents or dispersants, are preferably used to produce the sol or gel.
  • the solvent or dispersion medium has a weight-based ratio of water to organic solvent of 1:10 to 20: 1, in particular 1: 5 to 15: 1, preferably 1: 2 to 10: 1, preferably 1 : 1 to 5: 1, particularly preferably 1: 3.
  • the ratio of water to organic solvent can be used on the one hand to adjust the hydrolysis rate, in particular of the silicon-containing compound and of the alloying reagents, and on the other hand to adjust the solubility and reaction rate of the carbon-containing compound, in particular the carbon-containing precursor compound such as sugars.
  • the silicon-containing compound is selected from silanes, silane hydrolyzates, orthosilicic acid and mixtures thereof, in particular silanes.
  • orthosilicic acid and also its hydrolysis products can be obtained, for example, from alkali silicates whose alkali metal ions have been exchanged for protons by ion exchange.
  • alkali metal compounds are not used in the context of the present invention, since these, particularly when using a sol-gel process or when the sol is drying, the resulting precursor granules are incorporated and consequently can also be found in the compound containing silicon carbide.
  • alkali metal doping is generally not desired in the context of the present invention. If this should be desired, however, suitable alkali metal salts, for example the silicon-containing compound or also alkali phosphates, can be used.
  • silanes in particular tetraalkoxysilanes and / or trialkoxyalkylsilanes, preferably tetraethoxysilane, tetramethoxysilane or triethoxymethylsilane, are used as the silicon-containing compound in process step (i), since these compounds are hydrolysed to give orthosilicic acids or theirs Condensation products or highly cross-linked siloxanes and the corresponding alcohols react.
  • the carbon-containing compound is selected from the group of sugars, in particular sucrose, glucose, fructose, and invert sugar. sugar, maltose; Strength; Starch derivatives and organic polymers, especially phenol-formaldehyde resin, resorcinol-formaldehyde resin, and mixtures thereof.
  • sugars in particular sucrose, glucose, fructose, and invert sugar. sugar, maltose; Strength; Starch derivatives and organic polymers, especially phenol-formaldehyde resin, resorcinol-formaldehyde resin, and mixtures thereof.
  • the carbon-containing compound is used in an aqueous solution or dispersion.
  • the carbon-containing compound is usually introduced in a small amount of the solvent or dispersion medium, in particular water, provided for the processing of the precursor granules in process step (i).
  • the carbon-containing compound is used in a solution which contains the carbon-containing compound in amounts of 10 to 90% by weight, in particular 30 to 85% by weight, preferably 50 to 80% by weight , in particular 60 to 70% by weight, based on the solution or dispersion of the carbon-containing compound.
  • catalysts in particular acids or bases
  • the solution or dispersion of the carbon-containing compound for example in order to accelerate the inversion of sucrose and to achieve better reaction results.
  • process step (i) With regard to the temperatures at which process step (i) is carried out, it has proven useful if process step (i) at temperatures in the range from 15 to 40 ° C., in particular 20 to 30 ° C., preferably 20 to 25 ° C. , is carried out.
  • process step (ii) the temperatures are slightly increased in comparison to process step (i) in order to accelerate the reaction of the individual constituents of the solution or dispersion, in particular the condensation reaction when the sol ages to the gel .
  • process step (ii) is carried out at temperatures in the range from 20 to 80 ° C., in particular 30 to 70 ° C., preferably 40 to 60 ° C.
  • process step (ii) is carried out at 50 ° C.
  • time span for which process step (ii) is carried out this can vary depending on the respective temperatures, the solvents used and the precursor compounds used.
  • process step (ii) is usually carried out for a period of 15 minutes to 20 hours, in particular 30 minutes to 15 hours, preferably 1 to 10
  • the quantities of the individual components in process step (ii) can vary widely depending on the intended use.
  • the precursor compositions for stoichiometric silicon carbide or non-stoichiometric silicon carbides have completely different compositions and proportions of the individual components than compositions which are intended for the production of silicon carbide alloys.
  • the doping reagents or alloying reagents care must also be taken that they can be processed into homogeneous granules with a carbon source and a silicon source, which can react in generative manufacturing processes to form compounds containing silicon carbide.
  • the compounds used should have sufficiently high solubilities in the solvents used, in particular in ethanol and / or water, in order to be able to form finely divided dispersions or solutions, in particular brine, and should not be mixed with other components of the solution or during the production process the dispersion, especially the sol, react to form insoluble compounds.
  • the reaction rates of the individual reactions taking place must be coordinated with one another, since the hydrolysis, condensation and, in particular, the must run undisturbed in the run-up to the formation of granules.
  • the reaction products formed must furthermore not be sensitive to oxidation and, moreover, should not be volatile.
  • the solution or dispersion contains at least one doping and / or alloying reagent.
  • the solution contains a doping and / or alloying reagent
  • the solution or dispersion contains the doping or alloying reagent in amounts of 0.000001 to 60% by weight, in particular 0.000001 to 45% by weight .-%, preferably 0.000005 to 45 wt .-%, preferably 0.00001 to 40 wt .-%, based on the solution or dispersion.
  • the solution or dispersion has a doping reagent
  • the solution or dispersion has the doping reagent usually in amounts of 0.000001 to 0.5% by weight, preferably 0.000005 to 0.1% by weight, preferably
  • the solution or dispersion contains an alloy reagent
  • the solution or dispersion contains the alloy reagent in amounts of 5 to 60% by weight, in particular 10 to 45% by weight, preferably 15 to 45% by weight. , preferably 20 to 40 wt .-%, based on the solution or dispersion.
  • the doping reagent As far as the chemical nature of the doping reagent is concerned, it can be selected from the aforementioned compounds.
  • the alloy reagent is usually selected from compounds of Al, Ti, V, Cr, Mn, Co, Ni, Zn, Zr and their mixtures which are soluble in the solvent or dispersion medium.
  • the alloy reagent is selected from chlorides, nitrates, acetates, acetylacetonates and formates of Al, Ti, V, Cr, Mn, Co, Ni, Zn, Zr and mixtures thereof.
  • the solution or dispersion in the first process step contains the silicon-containing compound in amounts of 10 to 40% by weight, in particular 12 to 30% by weight. -%, preferably 15 to 25 wt .-%, preferably 17 to 20 wt .-%, based on the solution or dispersion.
  • the solution or dispersion contains the carbon-containing compounds in amounts of 6 to 40% by weight, preferably 8 to 30% by weight, preferably 10 to 25% by weight, particularly preferably 12 to 20 wt .-%, based on the solution or dispersion.
  • the solution or dispersion prefers the solvent or dispersant in amounts of 20 to 80% by weight, in particular 30 to 70% by weight, preferably 40 to 60% by weight 45 to 55 wt .-%, based on the solution or dispersion.
  • the solution or dispersion usually contains the doping reagent in amounts of 0.000001 to 0.5% by weight, preferably 0.000005 to 0.1% by weight, preferably 0.00001 to 0 , 01 wt .-%, based on the solution or dispersion. If a non-stoichiometric silicon carbide, in particular with a molar excess of silicon, is to be obtained, it has proven useful if the solution or dispersion in the first process step (a) contains the silicon-containing compound in amounts of 12 to 40% by weight, contains in particular 15 to 40% by weight, preferably 18 to 35% by weight, preferably 20 to 30% by weight, based on the solution or dispersion.
  • the solution or dispersion contains the carbon-containing compound in amounts of 6 to 40% by weight, preferably 8 to 30% by weight, preferably 10 to 25% by weight, particularly preferably 12 up to 20 wt .-%, based on the solution or dispersion.
  • the solution or dispersion in amounts of 20 to 80% by weight, in particular 30 to 70% by weight, preferably 40 to 60% by weight, preferably 45 to 55% by weight, based on the solution or dispersion.
  • the non-stoichiometric silicon carbide is to be doped, it has proven useful if the solution or dispersion contains the doping reagent in amounts of 0.000001 to 0.5% by weight, preferably 0.000005 to 0.1% by weight. , preferably 0.00001 to 0.01 wt .-%, based on the solution or dispersion.
  • the solution or dispersion in the first process step (a) contains the silicon-containing compound in amounts of 5 to 30% by weight, in particular 6 to 25% by weight, preferably 8 to Contains 20 wt .-%, preferably 10 to 20 wt .-%, based on the solution or dispersion.
  • the solution or dispersion contains the carbon-containing compound in amounts of 5 to 40% by weight, preferably 6 to 30% by weight, preferably 7 to 25% by weight, particularly preferably 10 to 20 wt .-%, based on the solution or dispersion.
  • the solution or dispersion contains the solvent or dispersion medium in amounts of 20 to 70% by weight, in particular 25 to 65% by weight, preferably 30 to 60% by weight, preferably 35 to Contains 50 wt .-%, based on the solution or dispersion.
  • the solution or dispersion contains the alloy reagent in amounts of 5 to 60% by weight, in particular 10 to 45% by weight, preferably 15 to 45% by weight, preferably 20 to 40% by weight, based on the solution or dispersion.
  • the alloy reagent is selected from the corresponding chlorides, nitrates, acetates, acetylacetonates and formates of the corresponding alloy elements.
  • process step (iii) As far as carrying out process step (iii) is concerned, it has proven useful if in process step (iii) the reaction product from process step (ii) at temperatures in the range from 50 to 400 ° C., in particular 100 to 300 ° C., preferably 120 to 250 ° C, preferably 150 to 200 ° C, is dried.
  • reaction product in process step (iii) is dried for a period of 1 to 10 hours, in particular 2 to 5 hours, preferably 2 to 3 hours.
  • reaction product it is possible for the reaction product to be comminuted in process step (iii), in particular after the drying process.
  • the reaction product is mechanically comminuted in process step (iii), in particular by grinding.
  • the grinding processes can be used to specifically set the particle sizes required or advantageous for carrying out additive manufacturing processes. However, it is often also sufficient to mechanically stress the reaction product from process step (ii) during the drying process, for example by stirring, in order to set the desired particle sizes.
  • a fourth process step (iv) following process step (iii) is preferably subjected to a reductive thermal treatment in the composition obtained in process step (iii), so that a reduced composition is obtained.
  • the use of a reduced composition which has been subjected to a reductive treatment has the advantage that a large number of possible and disruptive by-products have already been removed.
  • the resulting reduced precursor granulate is again significantly more compact and contains higher proportions of the elements that form the silicon carbide-containing compound.
  • process step (iii) If, after process step (iii), a reductive thermal treatment of the composition obtained in process step (iii) is carried out, it has proven useful if in process step (iv) the composition obtained in process step (iii) is heated to temperatures in the range from 700 to 1,300 ° C, in particular 800 to 1,200 ° C, preferably 900 to 1,100 ° C, is heated.
  • process step (iv) is heated for a period of 1 to 10 hours, in particular 2 to 8 hours, preferably 2 to 5 hours.
  • carbonization of the carbon-containing precursor material can take place, which can significantly facilitate the subsequent reduction, in particular of metal compounds.
  • Process step (iv) is generally carried out in a protective gas atmosphere, in particular in an argon and / or nitrogen atmosphere. This prevents the carbon-containing compound in particular from being oxidized.
  • the precursor compounds must not evaporate at the temperatures used of up to 1,300, preferably up to 1,100 ° C, but must be targeted under the reductive thermal conditions disintegrate into compounds which can be specifically converted into the desired silicon carbide-containing compounds during production.
  • the process for the preparation of a precursor granulate can also be carried out in such a way that
  • the implementation of a sol-gel process can often be dispensed with.
  • comparable precursor granules can often be obtained if the solvent or dispersion medium is removed after the formation of the sol, for example in vacuo.
  • the precursor granules obtained in this way can be converted into reduced precursor granules by temperature treatment in the range from 400 to 800 ° C.
  • the precursor granules obtained after the sol formation by removing the solvent or dispersant correspond in their percentage distribution of the elements contained to the precursor granules obtained by a sol-gel process and can be processed like these.
  • Fig. 4 shows an apparatus for performing the method according to the invention in an inkjet printing process
  • Fig. 5 shows a cross section through an apparatus for performing the method according to the invention in the form of a powder bed method
  • Fig. 6 is a sectional view of an apparatus for performing the method according to the invention as laser cladding
  • Fig. 7 shows a special embodiment of the device for performing the method according to the invention as laser cladding.
  • Another object of the present invention - according to a second aspect of the present invention - is a structured or surface-modified silicon carbide-containing object, in particular containing silicon carbide-containing material or consisting of silicon carbide-containing material, which is obtainable by the process described above.
  • the structured or surface-modified objects containing silicon carbide according to the invention are particularly evident in the fact that the object containing silicon carbide can either have different chemical compositions or have structured, in particular microstructured, surfaces.
  • Yet another object of the present invention - according to a third aspect of the present invention - is a device for performing the aforementioned method, the device
  • (b) has at least one device for generating laser beams, in particular at least one laser, for processing at least one substrate containing silicon carbide.
  • the silicon carbide-containing substrate can either be the finished silicon carbide-containing object or also intermediate stages during additive manufacturing.
  • the device for producing three-dimensional objects from materials containing silicon carbide by means of additive manufacturing is designed such that it has a device for generating laser beams, in particular at least one laser. With the aid of the laser, the precursor materials are then decomposed in a location-selective manner, so that materials containing silicon carbide are applied to a substrate surface in a location-selective manner and in layers.
  • the device for producing three-dimensional objects from silicon carbide-containing materials is preferably a device for selective synthetic crystallization, a device for carrying out printing processes, in particular inkjet processes, with subsequent laser-induced decomposition of the precursor materials or a device for laser deposition welding.
  • the device for carrying out the method also has at least one device for providing a layer of a precursor material or at least one device for applying precursor materials to a substrate or a device for generating a particle stream, in particular the precursor materials or their decomposition products.
  • the device according to the invention for generating laser beams for processing the surfaces of a substrate containing silicon carbide is based on conventional devices for laser ablation, but especially for the processing of silicon carbide-containing materials. This applies in particular to the lasers used.
  • the device according to the invention not only can ablation of surfaces containing silicon carbide be carried out, but it is also possible to manipulate the chemical modification of surfaces containing silicon carbide in a targeted manner, in particular by creating flaws on the surface by means of laser radiation and subsequent doping of the surface.
  • the surface of the silicon carbide-containing object or the partially produced silicon carbide-containing object is thermally treated with the device as part of the surface treatment, i.e. To be heated, it is often sufficient if the device has a device for generating laser beams, in particular the device for generating laser beams, which is used to carry out the additive manufacturing process.
  • the device if the device is to be used for ablation by means of a Coulomb explosion, the device usually has a plurality of, in particular at least two, devices for generating laser beams.
  • the device has means for contacting doping reagents with an optionally chemically modified surface of a material containing silicon carbide.
  • Such means can be, for example, as nozzles for spraying the chemically modified or activated surface of the substrate containing silicon carbide, in particular the object containing silicon carbide.
  • the doping reagents it is also possible for the doping reagents to be contained in the process atmosphere.
  • the device according to the invention it is in particular possible to specifically dope doped regions which have dimensions in one or two spatial directions of only a few micrometers.
  • a targeted subsequent doping of materials containing silicon carbide is also made possible.
  • the device has means for generating a process atmosphere, in particular an inert gas atmosphere, and / or means for generating a vacuum.
  • the method is usually carried out in an inert gas atmosphere or in a vacuum.
  • the device has devices for measuring the surface of the silicon carbide-containing material.
  • the device has an interferometer which registers the reflected laser beam and makes it possible to monitor the implementation of the method at the same time, ie in situ, and to monitor the laser power and the impact of the laser on the object containing silicon carbide or adapt the substrate specifically.
  • FIG. 1A shows sections of a simplified representation of the implementation of a method step of the method according to the invention in the form of an ablation.
  • the surface 1 of an object 2 containing silicon carbide which was produced by additive manufacturing in the form of layers 4, is irradiated by means of a laser beam 3 such that material is removed from the surface 1.
  • the material is removed either thermally by sublimation or by Coulomb explosion.
  • the material removal from the surface 1 of the silicon carbide-containing object 2 can be specifically adjusted by specifically controlling the laser power. In particular, it is also possible to process certain areas of the surface several times in order not to apply too much energy to the surface in one work step, and thus to effect material removal or change in areas in which this is not intended.
  • a precise removal of material in the nano- or micrometer range is possible, whereby in particular nano- and microstructuring of surfaces is possible, but also edges or contours of objects can be reworked.
  • FIG. 1B shows the implementation of a surface treatment carried out in the context of the method according to the invention by chemical modification of a surface 1 of an object 2 containing silicon carbide.
  • surface 1 of the object 2 containing silicon carbide is irradiated by means of a laser beam 3, preferably at temperatures in the range of 500 up to 1,800 ° C., whereby a change in the chemical structure of the silicon carbide-containing material in irradiated areas is obtained and a chemically modified area 5 is created.
  • a method for processing surfaces of materials containing silicon carbide is combined with additive manufacturing methods in the context of the present invention.
  • a surface 1 of an object 2 containing silicon carbide can be obtained by means of additive manufacturing and then the surface 1 can be processed by the action of laser radiation, either ablation or a chemical modification of the surface being carried out.
  • a further layer 4 of the silicon carbide-containing material can then be applied by means of additive manufacturing.
  • FIG. 2A and 2B show examples of application examples for the combination of additive and subtractive production, in particular for the processing of a silicon carbide-containing object 2 produced by means of additive production by means of ablation.
  • 2A shows an object 2 containing silicon carbide with a surface 1, which was built up with additive manufacturing in the form of layers 4.
  • the layer-by-layer structure of the silicon carbide-containing material 2 creates rough surfaces at the interface of the individual layers, which are due to the fact that a slight offset is formed between the individual levels can. Treatment of this uneven surface 1 by means of a laser beam 3 then results in a surface which is also flat in the micro or nanometer range.
  • FIG. 2B shows the geometric post-processing of an object 2 containing silicon carbide produced by means of additive manufacturing by ablation using a laser beam 3.
  • the silicon carbide-containing object 2 is built up layer by layer, in particular in the form of layers 4, and has a surface 1 which has a step-like structure due to the dissolution of the additive method used. Since a digital image, in particular a digital twin, of the silicon carbide-containing object 2 to be produced, the contour sharpness or resolution of which can be adjusted almost as desired, is preferably created before the silicon carbide-containing object 2 is set, the laser beam 3 can be used to easily and simply within the scope of the present invention Surface 1 of the silicon carbide-containing object 2 are reworked. 2B, the silicon carbide-containing object 2 is superimposed with the digital image and the laser beam 3 removes the material of the silicon carbide-containing object 2 along the cutting line specified by the projection 6 of the digital image.
  • the method according to the invention thus makes objects with a higher resolution and higher resolution accessible to silicon carbide than with pure additive methods.
  • FIG. 3 shows a silicon carbide-containing object 2 with a surface 1, which was successively built up by adding layers 4 by means of additive manufacturing.
  • Errors that occur during additive manufacturing or process-related lower resolutions can also be reworked immediately, so that surfaces with high contour sharpness are obtained.
  • the method according to the invention is preferably carried out using additive manufacturing methods which work with lasers. In this way it is often possible to use a laser to carry out both additive manufacturing and surface processing, in particular ablation or chemical modification of the surface.
  • FIG. 4 shows an example of a device 7 for producing silicon carbide-containing materials from liquid precursors, as is known from DE 10 2017 1 10 361 A1.
  • three-dimensional objects 2 containing silicon carbide with surfaces 1 can be created, which can be processed with laser beams 3.
  • the device 7 has a construction field 8 on which an object 2 made of silicon carbide-containing material is built.
  • the device 5 has in particular a discharge device 11 with discharge means 12, in particular one or more nozzles for the discharge of a solution or dispersion which contains precusors, in particular a precursor sol.
  • the construction site 8 or the discharge device 11 can be moved, in particular can be moved in an xy plane, preferably can be moved in the x, y and z directions. It is usually provided here that only the discharge device 11 or the construction field 8 can be moved.
  • the discharge device 11 can be moved in the xy plane, while the construction field 8 can be moved in the z direction, so that a layer-by-layer structure of the object 2 containing silicon carbide is made possible.
  • the discharge device 11, in particular the construction field 8, is designed in such a way that a solution or dispersion is applied to a substrate, in particular an object 2 containing silicon carbide or a construction field 8, by an ink jet printing process in a location-selective and locally limited manner.
  • the device 7 usually has means for generating laser beams 9, in which laser beams 3 are generated, and deflection means 10 for deflecting laser beams, in particular a mirror arrangement.
  • deflection means 10 for deflecting laser beams, in particular a mirror arrangement.
  • other structures are also possible, such as the means for generating laser beams and other means for aligning laser beams has, in particular z.
  • the procedure is preferably such that a solution or dispersion, which contains a suitable precursor, is applied to the construction field 8 or the silicon carbide-containing object 2 by means of the discharge device 11, in particular the application means 12, and then selectively by means of laser beams 3 is decomposed so that silicon carbide-containing materials are obtained.
  • an object 2 made of material containing silicon carbide can be obtained successively layer by layer by means of additive manufacturing.
  • the same means 9 for generating laser beams and the same deflection means 10, which are also used for additive manufacturing are preferably used for the surface processing.
  • the further means for generating laser beams are used specifically for surface processing, in particular for ablation or for the chemical modification of surface 1 of object 2 containing silicon carbide.
  • FIG. 5 shows a further variant of additive manufacturing, as is shown for example in DE 10 2017 1 10 362 A1.
  • an object 2 made of silicon carbide-containing material with a surface 1 is obtained by means of a powder bed process.
  • the device 7 shown in FIG. 5 likewise has means for generating laser beams 9 and deflection means for deflecting laser beams 10.
  • the device 7 has a construction field 8 on which the object 2 is produced from material containing silicon carbide.
  • a precursor material 13, in particular a powdery composition, is then, in particular distributed and selectively irradiated with laser beams 3 on the construction field 8 in order to obtain a layer of an object 2 containing silicon carbide.
  • a further precursor material 13 is distributed homogeneously and with a constant layer thickness on the construction field 8 from a storage device 14 by means of a distribution device 15 and this layer is again irradiated with laser beams 3 in a location-selective manner.
  • the construction area can in particular be moved in the z direction, preferably by means of a piston.
  • a three-dimensional object 2 made of silicon carbide-containing material is finally obtained by repeatedly carrying out the method described above.
  • surfaces 1 of the silicon carbide-containing material 2 are treated by means of ablation or chemical modification of the surface by irradiation of laser radiation 3 before the application of further layers.
  • the complete object is first produced and then the powder bed of precursor material 13 is removed before the surfaces 1 of the silicon carbide-containing object 2 are processed.
  • FIG. 6 shows a device 7 for the additive production of objects 2 containing silicon carbide by means of laser deposition welding.
  • the device 7 according to FIG. 6 has means 9 for generating laser beams 3 and at least one device 16 for generating a particle beam from gaseous, liquid or solid precursor materials 13.
  • the particle stream is preferably formed by powdered precursor materials 13.
  • the laser beams 3 and the particle stream of the precursor material 13 are directed onto the surface of a substrate 5 such that the laser beams 3 hit the particle stream in the immediate vicinity of the substrate surface.
  • the precursor materials 13 contained in the particle stream are decomposed or gasified, as a result of which reactive fragments are obtained and the desired silicon carbide material is deposited on the substrate surface in the form of an object 2 containing silicon carbide.
  • FIG. 7 shows an additive design of the device 7 for additive manufacturing by means of laser deposition welding.
  • FIG. 7 shows a section of a device 7.
  • the device 7 has a device 9 for generating laser beams, with which precursor materials 13 are gasified and decomposed - that can.
  • the device 7 according to this embodiment has devices 16 for generating a particle beam from preferably powdered precursor materials 13.
  • the devices 9 and 16 are integrated together in a preferably movable, in particular movable, device, in particular a nozzle head.
  • the device 7 also has, in particular, means 17 for generating a protective gas atmosphere, in particular a protective gas stream 18.
  • the protective gas stream 18 surrounds or surrounds the particle beam or the particle beams of the precursor material 13 and thus enables the precursor materials 13 to be decomposed in an inert gas atmosphere, in particular an argon atmosphere.
  • Alternative and equally preferred embodiments are not shown in the figures, in which different devices for generating laser beams, in particular pulse lasers, are used for additive manufacturing and subtractive manufacturing or chemical modification of the surface of silicon carbide-containing materials by means of laser radiation .
  • an ultrashort pulse laser in particular an excimer laser
  • the device 7 must have at least two different devices 9 for generating laser beams 3.

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Abstract

L'invention concerne un procédé de production et/ou de modification d'objets contenant du carbure de silicium.
EP20700189.2A 2019-01-18 2020-01-06 Procédé de production ou de modification d'objets contenant du carbure de silicium Withdrawn EP3911619A1 (fr)

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DE102019101268.6A DE102019101268A1 (de) 2019-01-18 2019-01-18 Verfahren zur Herstellung oder Modifizierung von siliciumcarbidhaltigen Objekten
PCT/EP2020/050118 WO2020148102A1 (fr) 2019-01-18 2020-01-06 Procédé de production ou de modification d'objets contenant du carbure de silicium

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US11459232B2 (en) * 2019-04-08 2022-10-04 Donna C. Mauro Additive manufacturing methods for modification and improvement of the surfaces of micro-scale geometric features
DE102020209386A1 (de) 2020-07-24 2022-01-27 Siemens Energy Global GmbH & Co. KG Verfahren zum Herstellen von Hohlräumen in einer schichtweise additiv herzustellenden Struktur
DE102021115402A1 (de) * 2021-06-15 2022-12-15 Fraunhofer Gesellschaft zur Förderung der angewandten Forschung e.V. Verfahren zur additiven Fertigung von Bauteilen, bei dem ein Bauteil durch Ablage mindestens eines Materials in Form von Tropfen hergestellt wird
DE112022003329T5 (de) * 2021-06-30 2024-04-11 Canon Kabushiki Kaisha Gegenstand, der siliciumcarbid als hauptbestandteil enthält, und verfahren zur herstellung desselben
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DE102022110873A1 (de) 2022-05-03 2023-11-09 Tdk Electronics Ag Additives Fertigungsverfahren mit Modifizierung von Teilschichten

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JP2022517637A (ja) 2022-03-09
WO2020148102A1 (fr) 2020-07-23
US20220097256A1 (en) 2022-03-31
DE102019101268A1 (de) 2020-07-23

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