EP2954372A2 - Ébauche en verre de tio2-sio2 pour un substrat de miroir, en vue d'une utilisation en lithographie euv, et son procédé de fabrication - Google Patents

Ébauche en verre de tio2-sio2 pour un substrat de miroir, en vue d'une utilisation en lithographie euv, et son procédé de fabrication

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Publication number
EP2954372A2
EP2954372A2 EP14702598.5A EP14702598A EP2954372A2 EP 2954372 A2 EP2954372 A2 EP 2954372A2 EP 14702598 A EP14702598 A EP 14702598A EP 2954372 A2 EP2954372 A2 EP 2954372A2
Authority
EP
European Patent Office
Prior art keywords
glass
sio
tio
temperature
blank
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Withdrawn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
EP14702598.5A
Other languages
German (de)
English (en)
Inventor
Stephan Thomas
Klaus Becker
Stefan Ochs
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.)
Heraeus Quarzglas GmbH and Co KG
Original Assignee
Heraeus Quarzglas GmbH and Co KG
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 Heraeus Quarzglas GmbH and Co KG filed Critical Heraeus Quarzglas GmbH and Co KG
Publication of EP2954372A2 publication Critical patent/EP2954372A2/fr
Withdrawn legal-status Critical Current

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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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
    • C03B19/1453—Thermal after-treatment of the shaped article, e.g. dehydrating, consolidating, sintering
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
    • C03B19/1469—Means for changing or stabilising the shape or form of the shaped article or deposit
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B25/00—Annealing glass products
    • C03B25/02—Annealing glass products in a discontinuous way
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/08—Mirrors
    • G02B5/0891—Ultraviolet [UV] mirrors
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/70—Microphotolithographic exposure; Apparatus therefor
    • G03F7/70216—Mask projection systems
    • G03F7/70316—Details of optical elements, e.g. of Bragg reflectors, extreme ultraviolet [EUV] multilayer or bilayer mirrors or diffractive optical elements
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/70—Microphotolithographic exposure; Apparatus therefor
    • G03F7/708—Construction of apparatus, e.g. environment aspects, hygiene aspects or materials
    • G03F7/7095—Materials, e.g. materials for housing, stage or other support having particular properties, e.g. weight, strength, conductivity, thermal expansion coefficient
    • G03F7/70958—Optical materials or coatings, e.g. with particular transmittance, reflectance or anti-reflection properties
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/20—Doped silica-based glasses doped with non-metals other than boron or fluorine
    • C03B2201/21—Doped silica-based glasses doped with non-metals other than boron or fluorine doped with molecular hydrogen
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/20—Doped silica-based glasses doped with non-metals other than boron or fluorine
    • C03B2201/23—Doped silica-based glasses doped with non-metals other than boron or fluorine doped with hydroxyl groups
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
    • C03B2201/40—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with transition metals other than rare earth metals, e.g. Zr, Nb, Ta or Zn
    • C03B2201/42—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with transition metals other than rare earth metals, e.g. Zr, Nb, Ta or Zn doped with titanium
    • 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
    • C03C2201/00—Glass compositions
    • C03C2201/06—Doped silica-based glasses
    • C03C2201/20—Doped silica-based glasses containing non-metals other than boron or halide
    • C03C2201/21—Doped silica-based glasses containing non-metals other than boron or halide containing molecular hydrogen
    • 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
    • C03C2201/00—Glass compositions
    • C03C2201/06—Doped silica-based glasses
    • C03C2201/20—Doped silica-based glasses containing non-metals other than boron or halide
    • C03C2201/23—Doped silica-based glasses containing non-metals other than boron or halide containing hydroxyl groups
    • 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
    • C03C2201/00—Glass compositions
    • C03C2201/06—Doped silica-based glasses
    • C03C2201/30—Doped silica-based glasses containing metals
    • C03C2201/40—Doped silica-based glasses containing metals containing transition metals other than rare earth metals, e.g. Zr, Nb, Ta or Zn
    • C03C2201/42—Doped silica-based glasses containing metals containing transition metals other than rare earth metals, e.g. Zr, Nb, Ta or Zn containing titanium
    • 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
    • C03C2203/00—Production processes
    • C03C2203/40—Gas-phase processes
    • 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
    • C03C2203/00—Production processes
    • C03C2203/50—After-treatment
    • C03C2203/52—Heat-treatment

Definitions

  • the present invention relates to a blank made of TiO 2 -SiO 2 glass for a mirror substrate for use in EUV lithography
  • the invention relates to a method for producing such a blank or a shaped body as a semi-finished product for its production.
  • EUV lithography highly integrated structures with a line width of less than 50 nm are produced by means of microlithographic projection devices.
  • laser radiation from the EUV range extreme ultraviolet light, also called soft x-ray radiation
  • the projection devices are equipped with mirror elements consisting of glass containing high-silica and titanium oxide (also referred to below as “TiO 2 - SiO 2 glass”), which are provided with a reflective layer system low linear coefficient of thermal expansion (referred to for short as "CTE", coef- ficient of thermal expansion), which can be set by the concentration of titanium.
  • CTE reflective layer system low linear coefficient of thermal expansion
  • Usual titanium oxide concentrations are between 6 and 9 wt .-%.
  • Such a blank made of synthetic, titanium-doped siliceous glass and a production method thereof are known from DE 10 2004 015 766 A1.
  • the TiO 2 -SiO 2 glass is produced by flame hydrolysis of titanium and silicon-containing starting substances and contains 6.8% by weight of titanium oxide. It is mentioned that the hydroxyl group content of the glass thus produced is 300% by weight. ppm rarely falls below.
  • To increase the radiation resistance of the glass it is proposed to lower the concentration of the hydrogen contained in the preparation by heating to values below 10 17 molecules / cm 3 . For this purpose, the glass is heated to a temperature in the range between 400 and 800 ° C and held at this temperature for up to 60 hours.
  • One of the plane surfaces of the mirror substrate is mirrored, wherein a plurality of layers is produced one above the other.
  • the maximum (theoretical) reflectivity of such an EUV mirror element is about 70%, so that at least 30% of the radiant energy in the coating or in the near-surface layer of the mirror substrate is absorbed and converted into heat.
  • the glass of the mirror substrate blank had a CTE which would be zero over the entire temperature range of the operating temperatures occurring in use.
  • the temperature range with a CTE around zero may be very narrow.
  • the temperature at which the thermal expansion coefficient of the glass is equal to zero is also referred to below as the zero-crossing temperature or as T Z c (temperature zero crossing).
  • the titanium concentration is usually adjusted to give a CTE of zero in the temperature range between 20 ° C and 45 ° C.
  • Volume ranges of the mirror substrate of higher or lower temperature than the preset T Z c expand or contract so that, despite the overall low CTE of the TiO 2 -SiO 2 glass, deformations occur under which the image quality of the mirror suffers.
  • WO 201 1/078414 A2 provides, in the case of a blank for a mirror substrate or for a mask plate made of SiO 2 -TiO 2 glass, to adjust the concentration of titanium oxide over the thickness of the blank stepwise or continuously to the temperature distribution which occurs during operation. that the condition for the zero-crossing temperature T Z c are fulfilled at each point, that is, the thermal expansion coefficient for the locally adjusting temperature is substantially equal to zero.
  • a CTE is defined as substantially equal to zero if the remaining linear expansion in operation at each point is 0 +/- 50ppb / ° C. This is to be achieved by varying the concentration of titanium- or silicon-containing starting substances in the production of the glass by flame hydrolysis in such a way that a predetermined concentration profile is established in the blank.
  • a projection lens contains a variety of mirrors of different size and shape, which not only have flat, but from convex or concave curved, mirrored surfaces with adapted to the specific use outer contours.
  • the actually occurring temperature profile over the volume of each component to be optimized during operation depends on the specific operating conditions and the environment and can be determined exactly only in the fully assembled projection objective under real operating conditions. The replacement of individual components of a ready mounted projection lens is technically hardly possible.
  • the CTE and thus scaling T Z c depend not only on the titanium oxide content but also on the hydroxyl group content and on the fictitious temperature of the glass.
  • the fictive temperature is a glass property that represents the ordered state of the "frozen" glass network.A higher fictitious temperature of the TiO 2 -SiO 2 glass is accompanied by a lower order state of the glass structure and a greater deviation from the most favorable structural arrangement.
  • the fictive temperature is determined by the thermal history of the glass, especially the last cooling process. In the process, different conditions inevitably result for near-surface regions of a glass block than for central regions, so that different volume regions of the mirror substrate blank already have different fictitious temperatures due to their different thermal history. The distribution of the fictive temperature over the blank volume is therefore always inhomogeneous. A certain equalization of the course of the fictitious temperature can be achieved by tempering. Annealing processes, however, are energy and time consuming.
  • the resulting fictitious temperature also depends on the composition of the TiO 2 -SiO 2 glass, and in particular on the hydroxyl group content and the titanium oxide concentration. Even by very careful and long tempering the course of the fictitious temperature on the blank volume can not be homogenized, if the composition is not completely homogeneous. However, this is not exactly the case with the hydroxyl group content, which can be changed by drying measures.
  • the invention has for its object to provide a blank for a mirror substrate of a TiO 2 -SiO 2 glass, in which the need for adaptation to optimize the course of CTE and thus the course of T Z c is low.
  • this object is achieved on the basis of a blank of the aforementioned type in that the TiO 2 - SiO 2 glass at a mean value of the fictitious temperature T f in the range between 920 ° C and 970 ° C, a dependence of its zero crossing temperature T.
  • Z c of the fictitious temperature T f which, expressed as a differential quotient dT Z c / dT f is less than 0.3.
  • TiO 2 -SiO 2 glasses show a decrease in CTE and an increase in T z c at the fictitious temperature.
  • This tangential slope according to the invention is less than 0.3, preferably less than 0.25, at any point within the fictitious temperature interval of 920 to 970 ° C.
  • Curve B shows, within the temperature interval from 920 to about 990 ° C at each point, a tangent slope of less than 0.3 expressed by the differential quotient dT Z c / dT f , whereas curve A does not show such a low point at any single point within that interval Slope shows.
  • the desired decoupling is achieved by a specific method for producing the TiO 2 -SiO 2 glass, which will be explained in more detail below.
  • the degree of decoupling of the dependence of the T Z c on the fictive temperature is to some extent dependent on the absolute level of the fictitious temperature itself. At low fictitious temperature, the desired decoupling easier than at high fictitious temperature succeed. The requirements are therefore higher, and the decoupling achieved is particularly noticeable when the notional temperatures of the blank are in the upper range of the temperature interval, for example, above 940 ° C.
  • the fictitious temperature again depends significantly on the same annealing treatment from the hydroxyl group content.
  • hydroxyl groups to achieve other, in particular optical or mechanical properties to some extent undesirable. As a suitable compromise between these other properties and a low fictive temperature, it has proven useful if the TiO 2 -SiO 2 glass has an average hydroxyl group content in the range of 200 to 300 ppm by weight.
  • the prerequisite for the setting of this average hydroxyl group content is the production of the TiO 2 -SiO 2 glass according to the so-called "soot method" obtained as an intermediate a porous soot body containing hydroxyl groups due to production. These can be removed by reactive chemical treatment by means of halogens to the desired extent. Preferably, however, the drying is carried out by thermal treatment of the soot body under vacuum.
  • OH content is determined by measuring the IR absorption by the method of D. M. Dodd et al. ("Optical Determinations of OH in Fused Silica", (1966), p. 391 1).
  • the TiO 2 -SiO 2 glass has an average hydrogen concentration of less than 5 ⁇ 10 16 molecules / cm 3 , preferably an average hydrogen concentration of less than 1 ⁇ 10 16 molecules / cm 3 .
  • the mean hydrogen concentration is determined by Raman measurements.
  • the measuring method used is described in: Khotimchenko et al., "De- termining the Content of Hydrogen Dissolved in Quartz Glass Using the Methods of Raman Scattering and Mass Spectrometry” Zhurnal Prikladnoi Spectroscopy, Vol. 46, No. 6 (June 1987), Pp. 987-991.
  • the mirror substrate blank according to the invention made of TiO 2 -SiO 2 glass is relatively insensitive to an inhomogeneous distribution of the fictive temperature over the volume of the blank.
  • the overall low thermal and spatial dependence therefore also facilitates the adaptation of the T Z c to an inhomogeneous temperature profile occurring in practice.
  • a further adaptation is provided in a preferred embodiment, in which the blank is delimited by a top side and a bottom side, wherein the TiO 2 -SiO 2 glass has a non-homogeneous course of the titanium oxide concentration between top side and bottom side.
  • the titanium oxide concentration of the glass is varied and thereby, for example, the T zc adapted to the operating temperature setting.
  • the blank is in this case designed as a composite body which comprises a first shaped body of TiO 2 -SiO 2 glass with a first titanium oxide concentration and a second shaped body of TiO 2 -SiO 2 glass with a second titanium oxide concentration. which is connected to the first molded body.
  • the moldings used as semifinished product consist of TiO 2 -SiO 2 glass according to the present invention, but with different titania concentration.
  • the moldings are joined together using known methods.
  • a higher fictitious temperature acts on the T Z c in the same manner as a higher titanium oxide concentration, that is, increasing T Z c for the respective TiO 2 -SiO 2 glass.
  • the fictitious temperature is also used to adapt the T zc to a predetermined temperature profile.
  • the first molded body has a first mean fictitious temperature and the second molded body has a second mean fictitious temperature, wherein the first and second fictitious temperature differ from each other.
  • the hydroxyl group content has an effect on the T zc and can be used as an additional parameter for adaptation to the given temperature profile.
  • the first and second shaped bodies are subjected to an annealing process prior to their connection, such that the fictitious temperatures that arise in the process differ from one another.
  • the moldings are plate-shaped with a maximum thickness of 60 mm.
  • a measured value averaged over the thickness is more meaningful in comparison to a measurement over the greater thickness of the complete mirror substrate blank.
  • the method for producing the blank according to the invention comprises the following method steps: (a) producing a first porous soot body of SiO 2 with a first concentration of titanium oxide by flame hydrolysis of silicon and titanium-containing starting substances,
  • the shaped body of TiO 2 -SiO 2 glass thus obtained can either be used directly as a mirror substrate blank after mechanical further processing, such as grinding and polishing, or it serves as a preliminary product for further processing into the blank.
  • the TiO 2 -SiO 2 glass produced in this way exhibits a CTE and a zero-crossing temperature Tzc, which are relatively insensitive to an inhomogeneous course of the notional temperature over the volume of the blank and therefore a relatively simple design to allow adaptation of the thermal expansion to a temperature profile which occurs in practical use over the thickness of the blank. This will be explained in more detail below:
  • the thermal expansion coefficient CTE and the zero-crossing temperature Tzc of TiO 2 -SiO 2 glass depend on the titanium concentration, the hydroxyl group content and the fictitious temperature. Since the fictive temperature is characterized by the thermal history of the glass, it is always inhomogeneous over the volume of the mirror substrate blank and can basically only be more or less aligned by energy-consuming and time-consuming tempering processes.
  • the method according to the invention makes it possible to produce a TiO 2 -SiO 2 glass which has a low dependency of CTE and T Z c on the fictitious temperature, so that a certain decoupling is achieved to that extent.
  • the mean hydroxyl group content of the TiO 2 -SiO 2 glass in the range from 200 to 300 ppm by weight can be adjusted during the production of the glass by the so-called "soot method".
  • a porous soot body is obtained, the hydroxyl groups in large quantities These can be removed by reactive chemical treatment by means of halogens, but preferably the drying is carried out by thermal treatment of the soot body under vacuum.
  • the soot method turns out to be disadvantageous in other respects.
  • the TiO 2 -SiO 2 glass obtained after vitrification is heated to a temperature at which the rutile microcrystals melt.
  • the glass is deformed and homogenized - for example, by twisting - to effect a more homogeneous distribution of TiO 2 -rich areas.
  • the TiO 2 -SiO 2 glass is subjected to a homogenization process in which it is heated to a temperature of more than 2000 ° C. and thereby softened and reshaped.
  • the high temperatures during the homogenization can cause a partial reduction of Ti 4+ in Ti 3+ .
  • the oxidation state of titanium oxide affects the coordination of the ion within the network structure, and that this change adversely affects the distribution of the titanium oxide - similar to the rutile formation. Therefore, according to the invention, during the homogenization at least at times an oxidatively acting atmosphere is set. In the area of the softened glass mass, an oxidizing gas, such as oxygen, is provided in excess and thus a partial reduction of Ti 4+ in Ti 3+ is counteracted.
  • the shaped bodies produced by process step (d) from the respective TiO 2 -SiO 2 glass exhibit a largely homogeneous distribution of titanium oxide with titanium in the tetravalent oxidation state.
  • the hydrogen contained in the preparation is reduced, so that in the TiO 2 -SiO 2 glass on average a very low hydrogen concentration of less than 5 ⁇ 10 16 molecules / cm 3 , preferably less than 1 adjusts x10 16 molecules / cm 3.
  • the TiO 2 -SiO 2 glass can be brought into a near-net shape, for example in plate form. Often, however, this shaping takes place in a separate shaping process.
  • the shaped body obtained by shaping exhibits a strongly inhomogeneous distribution of the fictitious temperature over its volume.
  • the shaped body is annealed. Annealing methods that are suitable for setting a fictitious temperature in this temperature range are to be developed by means of fewer and simpler tests.
  • the resulting fictive temperatures in the near-surface region of the top and bottom and the fictitious temperature in the volume (in the middle of the molding) differ from each other, the difference depending on the volume and thickness of the blank and at thicknesses 150 mm in the range of less degrees, typically around 5 ° C.
  • the TiO 2 -SiO 2 glass produced and reworked by means of the above-mentioned measures is characterized by a hydroxyl group content and a hydrogen concentration as specified above, and in particular by a zero crossing temperature Tzc, which lies in the interval between 920 ° C. and 970 ° C. To such a small extent depends on the fictitious temperature, as it was not previously known. This small dependence is expressed as the differential quotient dT Z c / dT f , which is less than 0.3.
  • the first TiO 2 -SiO 2 glass is preferably at least partially heated with a burner flame which contains fuel gas and at least one oxidizing gas. rende component are supplied in an excess amount for complete combustion of the fuel gas.
  • the burner flame a gas mixture of fuel gas and a fuel gas oxidizing component, in particular oxygen, burned.
  • a fuel gas oxidizing component in particular oxygen
  • the excess of oxidizing component in the gas mixture ensures that the fuel gas burns completely and that an excess remains which counteracts a partial reduction of titanium 4+ oxide.
  • the resulting decoupling of the T zc from the fictive temperature largely mitigates the problem of having to take into account the fictitious temperature as an influencing variable when adapting to an inhomogeneous course of the operating temperature which is set in use, and therefore simplifies this adaptation.
  • the adaptation to an inhomogeneous course of the operating temperature is preferably carried out by glass layers which differ in their titanium oxide concentration.
  • the glass layers are obtained by prefabricated, in particular plate-shaped moldings are joined together.
  • the prefabricated moldings are to be more accurately characterized by the usual measuring technique than the finished mirror substrate. So can the titania concentration and the CTE can be relatively easily measured optically or by ultrasonic measurement. However, a value averaged over the measuring path is obtained. In comparison with the measurement on the complete mirror substrate blank, the mean measured values are more meaningful when measured on the plate-like shaped bodies present in the intermediate stage.
  • the changes in the titanium dioxide concentration cause changes in the fictitious temperature; but these affect less than usual on the setting of T Z c.
  • the drying of the soot body is preferably carried out by heating the respective soot body under vacuum to a temperature of at least 1 150 ° C, preferably of at least 1200 ° C.
  • a high temperature shortens the treatment time required to remove the hydroxyl groups to a level in the range from 200 to 300 ppm by weight.
  • the homogenization according to method step (c) comprises a twisting, in which a cylindrical starting body made of the respective TiO 2 -SiO 2 glass held between two holders zonewise
  • the starting body is clamped in a equipped with one or more heating burners glass lathe and homogenized by means of a forming process, as described in EP 673 888 A1 for the purpose of complete removal of layers.
  • the starting body is locally heated to over 2000 ° C by means of a heating burner with an oxidizing burner flame and thereby softened.
  • the starting body is by relative movement of the two brackets twisted to each other around its longitudinal axis in several directions, the softened glass mass is thoroughly mixed.
  • a planar contact surface of the first mold body and a planar contact surface of the second mold body are assembled by wringing and welded together.
  • the bonding may comprise a joining step in which the upper mold resting on the second mold body is softened in an oven and deformed together therewith.
  • FIG. 1 shows a diagram for illustrating the temperature stratification in a mirror substrate with curved surfaces
  • Figure 3 is a diagram with derivatives (tangent slopes) of the specific
  • the diagram of Figure 1 shows the temperature distribution in a circular mirror substrate with curved surfaces, as in the thermal
  • the mirror substrate blank according to the invention shows a lower temperature dependency of the CTE on the fictive temperature, so that this adaptation effort is completely eliminated or at least less. This will be explained below by way of examples. Production of moldings with different titania concentration and fictitious temperature
  • Sample 1 a plate of TiO ? -SiO ? -Glass
  • octamethylcyclotetrasiloxane (OMCTS) and titanium isopropoxide [Ti (OPr ') 4 ] as a feedstock for the formation of SiO 2 -TiO 2 particles, a soot body made of synthetic TiO 2 -SiO 2 is prepared by the known OVD process 2 glass, which is doped with about 8 wt .-% TiO 2 .
  • the soot body is (cknen T Tro) at a temperature of 1 150 ° C in a heating furnace with a heating element of graphite in vacuum dehydrated.
  • the graphite in the furnace causes the setting of reducing conditions.
  • the dehydration treatment ends after 2 hours (t Tro ckn e n) -
  • the dried soot body is ( "2 mbar 10) vitrified in a sintering furnace at a temperature of about 1500 ° C under vacuum to a transparent blank of TiO 2 -SiO 2 glass.
  • the mean hydroxyl group content of the glass is at about 250 wt. ppm.
  • the glass is then homogenized by thermal mechanical homogenization (twisting) and formation of a cylinder of TiO 2 -SiO 2 glass.
  • a rod-shaped starting body is clamped in a glass lathe equipped with a oxyhydrogen burner and homogenized by means of a forming process, as described in EP 673 888 A1 for the purpose of complete removal of layers.
  • the starting material is locally heated to over 2000 ° C by means of the oxyhydrogen gas burner and thereby softened.
  • the oxyhydrogen gas burner to 1 mole of oxygen, 1, 8 mol of hydrogen supplied and thus produces an oxidizing oxyhydrogen flame.
  • the starting body By relative movement of the two brackets to each other, the starting body is twisted about its longitudinal axis, wherein the softened glass mass is intensively mixed to form a drill body in the radial direction.
  • An elongate drill body with a diameter of about 90 mm and a length of about 635 mm is obtained.
  • the drill body compressed to a ball-shaped mass, and the starting points of the brackets on the ball-shaped mass are displaced by 90 degrees.
  • This forming process is repeated until a blank homogenized in all dimensions is obtained.
  • the thus homogenized TiO 2 -SiO 2 glass is free of streaks in three directions, it contains no rutile microcrystals and shows a homogeneous titanium oxide concentration.
  • a round plate TiO 2 -SiO 2 glass is formed with a diameter of 30 cm and a thickness of 5.7 cm.
  • the glass plate is subjected to an annealing treatment.
  • the glass plate 8 hours during a holding time (t1 Te m em) under air and under atmospheric pressure at 1080 ° C (T1 Te m em) is heated and then (at a cooling rate of 4 ° C / h to a temperature of 950 ° C T2 Tem pern) and kept at this temperature for 4 hours (t2 Tem pern) long.
  • the TiO 2 -SiO 2 glass plate is cooled at a higher cooling rate of 50 ° C / h to a temperature of 300 ° C, whereupon the furnace is turned off and the glass plate is left to free cooling of the furnace.
  • the damaged surface layer of the glass plate is removed and a plan side is polished to give a diameter of 29.4 cm and a thickness d of 5.1 cm.
  • the plate thus obtained (sample 1a) consists of a particularly high-quality, homogenized, TiO 2 -SiO 2 glass which contains 7.7% by weight of titanium oxide.
  • the hydroxyl group content is 250 ppm by weight and for the hydrogen concentration an average value of 1 ⁇ 10 16 molecules / cm 3 is determined.
  • the mean fictive temperature measured over the entire thickness is 968 ° C.
  • sample 1 b and 1 c Two more glass plates are produced. The only difference lies in the tempering process. For sample 1b, t2 tem pern is shorter and for sample 1 c t2 Tem pern little longer than Probel.
  • the samples show the following average thickness measured fictitious temperatures:
  • the mean thermal expansion coefficient is determined interferometrically by the method described in: "R. Schödel, Ultra-high accuracy thermal expansion measurements with PTB's precision interferometer "Meas. Sei. Technol. 19 (2008) 084003 (1 1 pp)". From the CTE values measured in this way, the respective T Z c of the samples is computationally obtained in a known manner.
  • the diagram of Figure 2 shows the comparison of the two series of measurements.
  • the curve A combines the measured values of the samples of the commercially available TiO 2 -SiO 2 glass and the curve B the measured values of the samples 1 a, 1 b and 1 c for the TiO 2 -SiO 2 glass according to the invention.
  • the zero-crossing temperature T Z c (in ° C) is plotted against the measured fictitious temperature T f (in ° C).
  • the diagram of Figure 3 shows the derivatives of the curves A and B of Figure 2.
  • the differential quotient dT zc / dT f is plotted against the fictitious temperature T f .
  • the trace A shows a steeper course of T C z with the fictitious temperature.
  • the differential quotient dT zc / dT f at any point in the T r interval of 920 ° C. to 970 ° C. is less than 0.3 and only reaches this value at fictitious temperatures of less than 915 ° C. This shows the higher dependence of the T Z c on the fictive temperature in commercial TiO 2 -SiO 2 glass.
  • this lower sensitivity of the TiO 2 -SiO 2 glass prepared according to the invention not only allows a more precise, simple re and more homogeneous adjustment of the coefficient of thermal expansion within the molding, but also a structurally particularly simple adaptation of the mirror substrate blank to the T Z c-
  • Samples 2 and 3 further plates of TiO 2 -SiO 2 -glass As explained on the basis of sample 1 a, soot bodies of synthetic TiO 2 -SiO 2 glass are obtained by flame hydrolysis of OMCTS and titanium isopropoxide [Ti (OPr ') 4 ] produced different concentrations of TiO 2 . The concentrations are given in Table 1.
  • the soot bodies are dehydrated as sample 1 a each at a temperature of 1 150 ° C in a heating furnace with a heating element made of graphite under vacuum.
  • the dried soot body is vitrified into transparent blanks of TiO 2 -SiO 2 glass at about 1500 ° C under vacuum (10 "2 mbar).
  • the mean hydroxyl group content of the titanium-doped silica glass is in each case about 250 ppm by weight.
  • the glasses thus obtained are then further processed by thermal mechanical homogenization (twisting) under an oxidizing atmosphere.
  • Sample 2 is thereby homogenized in three directions (as explained with reference to sample 1 a, and this type of homogenization is referred to as "3D" in Table 1.)
  • Sample 3 was homogenized in the same way as samples 1 a and 2 under an oxidizing atmosphere, however in one direction only (in Table 1, this type of homogenization is referred to as 1D).
  • the round TiO 2 -SiO 2 glass plates formed from the blanks have a diameter of 30 cm and a thickness d of 5.7 cm (Sample 2) and 5.1 cm (Sample 3), respectively.
  • sample 2 these are subjected to the setting of a predetermined fictitious temperature of an annealing treatment. For sample 2, this corresponds approximately to that of sample 1 a (T2 Tempem for sample 2, however, is 930 ° C.).
  • the TiO 2 -SiO 2 glass plate is heated to 1080 ° C during a holding time of 8 hours under air and atmospheric pressure and then cooled at a cooling rate of 4 ° C / h to a temperature of 980 ° C and at this temperature Held for 4 hours. Thereafter, the TiO 2 -SiO 2 glass plate is cooled at a higher cooling rate of 50 ° C / h to a temperature of 300 ° C, whereupon the furnace is turned off and the plate is left to free cooling of the furnace.
  • the TiO 2 -SiO 2 glass of Sample 3 has an average fictitious temperature of 980 ° C.
  • soot bodies of synthetic TiO 2 -SiO 2 glass with different concentrations of TiO 2 are prepared by flame hydrolysis of OMCTS and titanium isopropoxide [Ti (OPr ') 4 ].
  • the concentrations are given in Table 1.
  • the soot body of Sample 4 is dehydrated like Samples 1 to 3. In the soot body of Sample 5, dehydration treatment is omitted.
  • the soot body be at about 1500 ° C under vacuum (10 "2 mbar) vitrified into transparent blanks of TiO 2 -SiO 2 glass.
  • the mean hydroxyl group content of TiO 2 -SiO 2 glass of Sample 4 is percent at about 250. ppm of sample 5 at 350 ppm by weight.
  • Sample 5 is then further processed by thermal mechanical homogenization (twisting).
  • the oxyhydrogen burner is operated during the entire process with stoichiometrically neutral flame, ie with a molar ratio of oxygen / hydrogen of 1: 2. Otherwise, the homogenization of sample 5 is carried out as described on the basis of sample 1a. For sample 4, homogenization is dispensed with.
  • both blanks are subjected to an annealing treatment, as described by sample 1 a. Thereafter, the TiO 2 -SiO 2 glass of Sample 4 has an average fictitious temperature of 967 ° C and that of Sample 5 has an average fictitious temperature of 952 ° C due to its higher hydroxyl group content.
  • sample 6 corresponds to the commercially available TiO 2 -SiO 2 glass on which the measurement curve A of FIG. 2 is based.
  • the values of the "?” Provided manufacturing parameters are unknown for this glass.
  • Each of Samples 1 to 3 can be used by itself as a mirror substrate blank with little deformation at an inhomogeneous temperature course readily.
  • the melted composite is tempered to remove mechanical stress.
  • the temperature profile when annealing the melt-bonded body is as follows: heating to a temperature of 1080 ° C, holding at that temperature for a holding time of 10 hours; Cooling at a cooling rate of 4 ° C / h to a temperature of 950 ° C and held at that temperature for a period of 12 hours, followed by free cooling to room temperature.
  • the mirror substrate blank produced in this way is composed of only two components of different chemical composition, namely the upper shaped body of sample 1 and the lower shaped body of sample 2. These are connected to one another via a substantially flat and planar contact surface.
  • the mirror substrate blank is used to produce a mirror substrate made of titanium-doped glass for use in EUV lithography.
  • the top surface of the mirror substrate blank formed by sample 1 which faces the EUV radiation when it is used as intended, is subjected to a mechanical treatment which comprises grinding and polishing.
  • the contour of the mirror is generated as a concavely curved surface area.
  • Comparative Example 1 In order to adapt the T Z c to a temperature profile as shown in FIG. 1, a mirror substrate blank of two layers is built up using the procedure described in Example 1. In contrast, instead of Sample 1, Sample 4 is used. The method of preparation of sample 4 is similar to that of sample 1, but it is not homogenized. This adaptation of the T Z c is not sufficient to ensure a small deformation of the mirror substrate as a whole at the predetermined temperature profile. The remaining length expansion in operation is in places above 0 +/- 20ppb / ° C.

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Abstract

L'objectif de la présente invention est de préparer une ébauche en verre de TiO2-SiO2 pour un substrat de miroir, en vue d'une utilisation en lithographie EUV, de manière que le besoin d'adaptation pour optimiser la courbe du coefficient de dilatation thermique et ainsi aussi la courbe de la température de passage par zéro Tzc est faible. A cette fin, lorsque la température fictive Tf présente une valeur moyenne située entre 920°C et 970°C, la température de passage par zéro Tzc du verre de TiO2-SiO2 est fonction de la température fictive Tf qui, exprimée comme dérivée dTzc/dTf, est inférieure à 0,3.
EP14702598.5A 2013-02-11 2014-02-04 Ébauche en verre de tio2-sio2 pour un substrat de miroir, en vue d'une utilisation en lithographie euv, et son procédé de fabrication Withdrawn EP2954372A2 (fr)

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DE102013101328.7A DE102013101328B3 (de) 2013-02-11 2013-02-11 Rohling aus TiO2-SiO2-Glas für ein Spiegelsubstrat für den Einsatz in der EUV-Lithographie sowie Verfahren für dessen Herstellung
PCT/EP2014/052106 WO2014122111A2 (fr) 2013-02-11 2014-02-04 Ébauche en verre de tio2-sio2 pour un substrat de miroir, en vue d'une utilisation en lithographie euv, et son procédé de fabrication

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EP2960219B1 (fr) * 2014-06-27 2019-01-16 Heraeus Quarzglas GmbH & Co. KG Ebauche en verre de quartz doté de titane pour un substrat de miroir à utiliser dans la lithographie EUV et son procédé de fabrication
WO2016044952A1 (fr) 2014-09-25 2016-03-31 Suzhou Synta Optical Technology Co., Ltd. Procédé de fabrication d'ébauches de miroir de télescope de grande taille et léger et ébauches de miroir fabriquées selon celui-ci
WO2016086013A1 (fr) * 2014-11-26 2016-06-02 Corning Incorporated Procédé de fabrication d'un élément optique dopé avec un halogène
CN111238461B (zh) * 2020-03-09 2022-05-06 中国建筑材料科学研究总院有限公司 一种谐振子及其制备方法
CN113340504B (zh) * 2021-07-13 2022-03-01 中国工程物理研究院激光聚变研究中心 一种从熔石英假想温度分布获取残余应力分布的方法
CN113737278B (zh) * 2021-07-29 2022-05-03 达高工业技术研究院(广州)有限公司 氧化钛掺杂旋涂玻璃固化装置

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WO2014122111A3 (fr) 2014-10-23
KR101922765B1 (ko) 2018-11-27
US20150376049A1 (en) 2015-12-31
WO2014122111A2 (fr) 2014-08-14
TW201446670A (zh) 2014-12-16
KR20150117675A (ko) 2015-10-20
CN104995557A (zh) 2015-10-21
US9522840B2 (en) 2016-12-20
DE102013101328B3 (de) 2014-02-13
JP6328665B2 (ja) 2018-05-23
JP2016511211A (ja) 2016-04-14
TWI624435B (zh) 2018-05-21

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