Classifications

• • C—CHEMISTRY; METALLURGY
  • C03—GLASS; MINERAL OR SLAG WOOL
  • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
  • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
  • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
  • C03C17/23—Oxides
  • C03C17/25—Oxides by deposition from the liquid phase
• • C—CHEMISTRY; METALLURGY
  • C03—GLASS; MINERAL OR SLAG WOOL
  • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
  • C03B19/00—Other methods of shaping glass
  • C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
  • C03B19/066—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction for the production of quartz or fused silica articles
• • C—CHEMISTRY; METALLURGY
  • C03—GLASS; MINERAL OR SLAG WOOL
  • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
  • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
  • C03C17/02—Surface treatment of glass, not in the form of fibres or filaments, by coating with glass
• • C—CHEMISTRY; METALLURGY
  • C03—GLASS; MINERAL OR SLAG WOOL
  • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
  • C03C2217/00—Coatings on glass
  • C03C2217/20—Materials for coating a single layer on glass
  • C03C2217/21—Oxides
  • C03C2217/213—SiO2
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T428/00—Stock material or miscellaneous articles
  • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension

Definitions

• the invention relates to a method for producing a coated component made of quartz glass by at least partially covering the surface of a base body made of quartz glass with a SiO 2 glass mass which differs in its optical, physical or chemical properties from the quartz glass of the quartz glass Base body is different.
• Quartz glass is characterized by a low coefficient of expansion, by optical transparency over a wide wavelength range and by high chemical and thermal resistance. Quartz glass components are used for a variety of applications, such as in Lampenfer ⁇ tion as cladding tubes, pistons, cover plates or reflector support for lamps and radiators in the ultraviolet, infrared and visible spectral range, or in semiconductor manufacturing in the form of reactors and apparatus made of quartz glass for the treatment of semiconductor components, carrier shelves, bells, crucibles, protective shields or simple quartz glass components, such as tubes, rods, plates, flanges, rings or blocks. To produce special properties, quartz glass is doped with other substances.
• the quartz glass components are exposed to high thermal loads and chemically aggressive environments.
• a good heat insulation, a high temperature stability or thermal shock resistance as well as a high chemical resistance and freedom from contamination play an important role.
• Increasingly higher demands are placed on the service life of such quartz glass components.
• semiconductor fabrication processes such as sputtering or vapor deposition processes, often have the problem that material layers are deposited on all surfaces within the reactor, and in particular also on the surfaces of the quartz glass.
• the layers of material can come off with the material and then lead to particle problems.
• the corresponding quartz glass surfaces are cleaned from time to time, which usually takes place by etching with a fluorine-containing medium, in particular by means of hydrofluoric acid.
• the cleaning process is not only time-consuming and expensive, but also leads to a removal of quartz glass and a gradual reduction in the wall thickness of the quartz glass components. This also limits the life of the components concerned.
• the glazed, transparent surface layer acts as a heat insulator, which makes sufficient heating of the layers underneath difficult.
• This problem can not be solved by higher flame temperatures, as these lead to a plastic deformation of the component and evaporation of gaseous silicon monoxide (SiO).
• the object of the invention is to provide a cost-effective component made of quartz glass, in particular for use in semiconductor production, which is distinguished by high purity, high etching resistance (and thus a long service life), and which produces as few particle problems as possible.
• this object is achieved on the basis of the method mentioned above in that an amorphous slip containing SiO 2 particles is produced and applied to the surface of the base body to form a slip layer, the slip layer is dried and then dried is vitrified to form the SiO 2 -Glasmasse.
• the SiO 2 particles consist of synthetically produced SiO 2 or of purified naturally occurring raw material, as described in the above-mentioned DE 4440 104 C2.
• the drying of the slip layer is carried out by removal of moisture at room temperature, by heating or by freeze-drying.
• the slip layer is vitrified by heating to a high temperature which results in sintering of the SiO 2 particles and formation of a dense, crack-free glass mass of opaque, partly opaque, and partly transparent or completely transparent SiO 2 , and which covers the entire surface of the base body or a part thereof.
• the SiO 2 glass mass is in the form of an even layer or it forms a shape which constitutes a functional constituent of the component, for example as a thickening or bulge.
• the base body is a body of quartz glass made of synthetically produced or naturally occurring raw materials.
• the quartz glass of the base body may be transparent or opaque (translucent).
• SiO 2 particles are used for the formation of the glass mass, the particle size in the range up to a maximum of 500 .mu.m, preferably at most 100 .mu.m, wherein SiO 2 particles with particle sizes in the range between 1 .mu.m and 50 .mu.m account for the largest volume fraction.
• the cristobalite content in the dried SiO 2 slurry layer should be at most 1% by weight, otherwise crystallization may occur during vitrification of the slurry layer, which may result in rejection of the component.
• Roughening the surface of the base body causes better adhesion of the slurry layer as well as the SiO 2 glass mass produced therefrom by vitrification.
• the roughening is done mechanically (for example by grinding or sandblasting) or chemically (by etching), the surface should have a mean roughness R a of at least 0.5 microns.
• the known per se processing techniques are suitable, such as spraying, electrostatically assisted spraying, Flu ⁇ th, spin, dipping, printing, drawing and stripping (Doctor Blade method) or brushing.
• the SiO 2 particles are amorphous, produced by wet grinding of SiO 2 exit flow in the liquid, and particle sizes in the casting Have a maximum range of 500 microns, with SiO 2 particles having particle sizes in the range between 1 .mu.m and 50 .mu.m make up the largest Volumen ⁇ share, and that the green body is compacted by heating in a hydrogen-containing atmosphere.
• vitrification takes place under reducing conditions by heating the green body in a hydrogen-containing atmosphere.
• the green body is thermally solidified and at least the surface in the form of a SiO 2 -Glas mass completely ver ⁇ glazed.
• the hydrogen during sintering ensures rapid temperature compensation between the higher temperature applied to the surface and the lower temperature in the interior of the green body.
• the resulting particularly low temperature gradient despite a comparatively low maximum temperature in the region of the surface (which does not yet effect complete dense sintering), facilitates a progression of the enamel front from outside to inside.
• the cristobalite content of the starting material should be at most 1% by weight (based on the dry mass of the green body).
• the amorphous SiO 2 particles preferably have particle sizes in the range up to a maximum of 50 ⁇ m during casting. Smaller particles are characterized by a higher sintering activity and facilitate complete vitrification of the layer.
• Such a SiO 2 glass mass is obtained by applying a mass of SiO 2 particles containing slip on the surface of the base body, and by subsequent drying and vitrification of the mass, as explained in more detail above for the inventive method.
• the SiO 2 glass mass consists entirely or for the most part of SiO 2 , which has been prepared and applied by means of the slip process, and completely or only partly covers the component surface. It forms a planar layer on the component surface or contributes to the geometric shape of the component and forms a functional component of the component, for example a thickening or a bead, which can serve as a flange or ground part, for example. So- far a smooth and dense surface is required, this is preferably obtained by Feuerpolitur.
• the definition of the surface roughness R a results from EN ISO 4287, the measurement conditions from EN ISO 4288 (here, the case of a non-periodic surface profile is present).
• the mean surface roughness R 3 of the SiO 2 glass mass is at least 0.5 ⁇ m, preferably at least 1.0 ⁇ m. It has proved to be advantageous if the SiO 2 glass mass in relation to the base body consists of species-specific material.
• the SiO 2 glass mass may be opaque, partially opaque and transparent or completely transparent.
• FIG. 4 shows a semifinished product for producing a spherical grinding in a schematic representation.
• This mixture is ground by means of milling balls made of quartz glass on a roller block at 23 U / min for a period of 3 days so far that a homogeneous base slip having a solids content of 79%.
• milling balls made of quartz glass on a roller block at 23 U / min for a period of 3 days so far that a homogeneous base slip having a solids content of 79%.
• the Milling occurs as a result of the going into solution SiO 2 to a lowering of the pH to about 4.
• Example 2 The prepared on the basis of Example 1 and dried slurry layer on the quartz glass flange is then vitrified under pure hydrogen atmosphere an ⁇ hand of the heating profile shown in Figure 2 in a sintering furnace.
• a crack-free and transparent SiO 2 layer is obtained, which is distinguished by a particularly low bubble content and whose characteristics and quality otherwise correspond to the layer 31 described above with reference to FIG.
• the bead-like thickened slip layer produced and dried using Example 2 at the end of the quartz glass tube is subsequently vitrified by means of a oxyhydrogen gas burner.
• the thickening is heated until a completely transparent, flame-polished and dense surface is obtained.
• a slip layer is produced on a rod of transparent, synthetically produced quartz glass having a hydroxyl group content of 250 ppm by weight by immersion and then dried as described in Example 1. After drying, the thickness of the slurry layer is 0.3 mm. Glazing takes place in an oven under air, the heating profile corresponding to that shown in FIG. 2 and explained in greater detail above in Example 3, but with the difference that the holding time is two hours at the maximum temperature of 1400 ° C. eliminated. The cooling starts immediately after this temperature is reached.
• the dried slurry layer produced on the quartz glass rod produced with the aid of Example 6 is introduced into a sintering furnace for vitrification, where it is glazed in air.
• the heating profile corresponds to that as shown in Figure 2 and above Toggle handle Example 3 is explained in more detail, with the difference that the temperature is not Maximaltempe ⁇ 1400 0 C, but only 1050 0 C. At this temperature, the coated silica glass rod is held for 2 hours and then cooled.
• the resulting SiO 2 glass mass shows a high density of about 2.15 g / cm 3 , but is still substantially opaque.
• the opacity is shown by the fact that the direct spectral transmission in the wavelength range between 190 nm and 2650 nm is below 10%.
• a green body 20 is produced from the homogeneous slip 14.
• the slip 14 is poured into a tubular membrane mold of vacuum-formed silicone, which is embedded in carbon dioxide snow (dry ice). This causes a rapid freezing of the slurry 14 to a blue body 22 in the form of a rod with an outer diameter of 10 mm.
• the addition of glycerine contributes to a homogeneous structure that is free of iron needle structures.
• the shock-frozen Blue body 22 is removed from the membrane and directly form - introduced in an air oven preheated to 80 0 C and environmental therein for several hours at this temperature dried Tem ⁇ - in a frozen state. Continuous evaporation and removal of moisture from the surface will prevent recondensation of moisture and re-surface freezing, which would be associated with needle crystal formation and disruption of the green body structure.

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• Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• Materials Engineering (AREA)
• Organic Chemistry (AREA)
• Geochemistry & Mineralogy (AREA)
• Life Sciences & Earth Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Manufacturing & Machinery (AREA)
• Dispersion Chemistry (AREA)
• Glass Melting And Manufacturing (AREA)
• Glass Compositions (AREA)
• Surface Treatment Of Glass (AREA)

Priority Applications (4)

Applications Claiming Priority (4)

Publications (2)

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Family Applications (1)

Country Status (5)

Cited By (5)

Families Citing this family (24)

Family Cites Families (19)

• 2004
  • 2004-10-28 DE DE102004052312A patent/DE102004052312A1/de not_active Withdrawn
• 2005
  • 2005-08-23 JP JP2007528725A patent/JP2008510676A/ja active Pending
  • 2005-08-23 WO PCT/EP2005/009073 patent/WO2006021415A2/de not_active Ceased
  • 2005-08-23 EP EP05781997.1A patent/EP1789370B1/de not_active Expired - Lifetime
  • 2005-08-23 EP EP10182969.5A patent/EP2263981B1/de not_active Expired - Lifetime
  • 2005-08-23 US US11/661,160 patent/US20080075949A1/en not_active Abandoned

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