Classifications

• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
  • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
  • C23C14/067—Borides
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
  • B22F3/12—Both compacting and sintering
  • B22F3/14—Both compacting and sintering simultaneously
  • B22F3/15—Hot isostatic pressing
• • C—CHEMISTRY; METALLURGY
  • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
  • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
  • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/515—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
  • C04B35/58—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
  • C04B35/5805—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides
  • C04B35/58064—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides
  • C04B35/58071—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides based on titanium borides
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
  • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
  • C23C14/34—Sputtering
  • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
  • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
• • C—CHEMISTRY; METALLURGY
  • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
  • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
  • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
  • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
  • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
  • C04B2235/38—Non-oxide ceramic constituents or additives
  • C04B2235/3804—Borides
  • C04B2235/3813—Refractory metal borides
• • C—CHEMISTRY; METALLURGY
  • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
  • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
  • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
  • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
  • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
  • C04B2235/54—Particle size related information
  • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
  • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron

Definitions

• the invention relates to a titanium diboride target for the physical
• PVD processes are coating processes in which the coating is physically removed by vaporization of the layer-forming particles from a target
• PVD processes are also increasingly used for the production of hard coatings in tools for machining or wear parts.
• various PVD methods have
• the targets for better temperature distribution are often provided with a rear-side cooling plate, which is either in positive contact with the target in good thermal contact or even connected by a suitable bonding method cohesively with the target.
• the ARC PVD method has compared to the
• Sputtering process the advantage that higher ionization rates and higher deposition rates can be achieved.
• the process is thereby more economical, the process control improved and the higher energetic growth conditions make it possible to positively influence the layer structure.
• Titanium diboride which are often used as hard material layers, which come into contact with non-ferrous metals due to their high hardness and above all good wear resistance, are by means of
• Titanium diboride has a low thermal shock resistance. Due to the ARC PVD process, the target only evaporates in very narrow spatial and temporal zones due to the arc. Due to these properties of the titanium diboride, large thermal stresses occur and the target can be destroyed prematurely.
• Titanium diboride layers using these ARC evaporation sources using these ARC evaporation sources.
• Production of titanium diboride targets is to make coatings over the
• the titanium diboride targets prepared in this way still do not have the necessary thermal shock resistance, which would be necessary for a smoothly functioning ARC PVD coating process in practice.
• Object of the present invention is therefore to provide a titanium diboride target, which can be used without problems in practice for the ARC coating process. According to the invention this is achieved in that the mean grain size of the titanium diboride grains is between 1 pm and 20 m, the carbon content is in a range of 0.1 to 5 wt.%, The total content of iron, nickel, cobalt and / or chromium is in the range of 500 to 3000 pg / g and the carbon is distributed in free form at the grain boundaries of the titanium diboride grains so that the average distances between the individual
• Carbon particles are smaller than 20 pm and that the porosity is less than 5 vol.%.
• the mean grain size of the titanium diboride grains is determined by the
• titanium diboride targets Due to the present invention, it has been found that by a completely uniform carbon distribution and distribution of the metallic additives within the specified ranges titanium diboride targets are created, which can be evaporated easily with the ARC PVD process without it due to thermal stresses to a local or complete bursting of the target comes.
• This is achieved by milling a starting powder mixture of TiB 2 powder and graphite powder in a grinding unit with grinding balls containing one or more metals from the group Fe, Ni, Co and Cr until the total content of Fe, Ni, Co and / or Cr in the range of 500 to
• Powder mixing by hot pressing at a pressure in the range of 10 MPa to 40 MPa and at a temperature in the range of 1,600 ° C to 2,000 ° C, takes place. It is important that the metallic components are not added as a powder, but only as abrasion on the grinding balls, which contain at least one of the metals listed, are introduced.
• Starting powder mixture of TiB 2 powder and graphite powder is ground in an attritor with iron balls, until the iron content is in the range of 500 to 3000 g / g and compressing the ground powder mixture by hot pressing, at a pressure in the range of 25 to 35 MPa and a temperature in the range of 1650 ° C to 1850 ° C, takes place.
• the grinding process essentially serves the uniform distribution of the carbon and the metallic components. Typical meals with which the metallic additives are incorporated within the specified range, depending on the type of mill used on the order of 10 to 120 minutes. A particularly rapid introduction is by the
• hot pressing in the context of the present invention is intended to include all variants of hot pressing with or without direct current passage such as the SPS method (spark pjasma sintering) or
• FAST field assisted sintering
• a round-shaped target was 60 mm
• Diameter and 8 mm thickness produced according to the invention.
• the starting material used was a titanium diboride powder having a boron content of 30.88% by weight, an iron content of 0.023% by weight, a carbon content of 0.020% by weight, the remainder titanium, with a mean particle size d 50 of 2.39 ⁇ m.
• FIG. 1 shows the scanning electron micrograph
• Example 1 For purposes of comparison, a target of the same dimensions as in Example 1 was made with similar preparation parameters but not according to the invention without the addition of carbon.
• the starting material used was a titanium diboride powder having a boron content of 31, 71% by weight, an iron content of 0.032% by weight, a carbon content of 0.044% by weight, the remainder titanium, with a mean particle size d 50 of 4.48 ⁇ m.
• the powder was compacted in a hot press at a maximum pressing pressure of 30 MPa and a maximum temperature of 1,800 ° C with a holding time of 20 min.
• the starting material was a titanium diboride powder having a boron content of 31.4% by weight, an iron content of 0.028% by weight, a carbon content of 0.042 wt.%, Balance titanium, used with a mean particle size d 50 of 3.81 pm.
• the starting powder was in a hot press once with a maximum pressing pressure of 30 MPa and a maximum temperature of 1,800 ° C with a holding time of 60 min and once with a maximum pressing pressure of 30 MPa and a maximum temperature of 2200 ° C with a holding time of Compressed for 30 minutes.
• the hot pressing achieved a target with a density of the material of 3.3 g / cm 3 , which corresponds to 73% of the theoretical density, and in the second case a target with a density of the material of 3.4 g / cm 3 , which corresponds to 76% of the theoretical density.
• the targets prepared according to Example 3 were already destroyed during processing for installation in the cathode holder and therefore could not be used.
• the target produced according to the invention according to Example 1 has behaved stably in a 60 minute operation.
• the target did not show any cracks and showed a smooth surface removed by 1 to 2 mm in thickness.
• the target not according to the invention produced according to Example 2 has already been torn after a few minutes of operation and soon after completely destroyed.
• the targets prepared according to Comparative Examples 2 and 3 clearly show that both the addition of carbon and the uniform distribution of small amounts of iron, which are introduced exclusively by abrasion during grinding into the starting powder, are necessary for good functionality of the invention To ensure targets.
• targets are also included, which are connected in a material-bonded manner by a bonding method to a cooling plate made of molybdenum, for example.

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• Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• Organic Chemistry (AREA)
• Materials Engineering (AREA)
• Mechanical Engineering (AREA)
• Metallurgy (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Manufacturing & Machinery (AREA)
• Ceramic Engineering (AREA)
• Structural Engineering (AREA)
• Physical Vapour Deposition (AREA)
• Powder Metallurgy (AREA)
• Hybrid Cells (AREA)

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• 2010
  • 2010-05-04 AT AT0028810U patent/AT11884U1/de not_active IP Right Cessation
• 2011
  • 2011-05-02 WO PCT/AT2011/000209 patent/WO2011137472A1/de not_active Ceased
  • 2011-05-02 US US13/696,117 patent/US9481925B2/en active Active
  • 2011-05-02 EP EP11726642.9A patent/EP2567000B1/de active Active
  • 2011-05-02 RU RU2012144268/02A patent/RU2561624C2/ru not_active IP Right Cessation
  • 2011-05-02 CN CN201180021702.2A patent/CN102869807B/zh active Active
  • 2011-05-02 JP JP2013508328A patent/JP5815678B2/ja active Active

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