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US20020081465A1 - Sputtering targets and method for the preparation thereof - Google Patents

Sputtering targets and method for the preparation thereof Download PDF

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Publication number
US20020081465A1
US20020081465A1 US09/966,636 US96663601A US2002081465A1 US 20020081465 A1 US20020081465 A1 US 20020081465A1 US 96663601 A US96663601 A US 96663601A US 2002081465 A1 US2002081465 A1 US 2002081465A1
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titanium dioxide
target
plasma
argon
sputtering
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US09/966,636
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Johan Vanderstraeten
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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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • 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
    • 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
    • C03C17/245—Oxides by deposition from the vapour phase
    • C03C17/2456—Coating containing TiO2
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
    • C23C4/11—Oxides
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • C23C4/134—Plasma spraying
    • 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
    • C03C2217/212—TiO2
    • 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
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/15—Deposition methods from the vapour phase
    • C03C2218/154—Deposition methods from the vapour phase by sputtering

Definitions

  • the present invention relates to improved sputtering targets and, in particular to sputtering targets of titanium dioxide, and to a method for the preparation thereof.
  • Sputtered coatings of various oxides e.g. silica
  • nitrides e.g. silicon nitride
  • optical coatings showing interesting properties on a number of substrates.
  • Known applications include low emissivity films on window glasses, cold mirrors on reflectors, enhanced mirrors for photocopiers and antireflective coatings on picture glass or TV screens.
  • These coatings are usually made of stacks of several different layers with different refractive indices, preferably of low and high refractive index, to produce optical filters.
  • refractive indices preferably of low and high refractive index
  • antireflective coatings it is preferred to combine two materials showing the highest and the lowest possible refractive indices. Such materials are titania and silica. Another advantage of these materials is their durability.
  • Titanium dioxide coatings have a high refractive index and can thus be used to provide coatings of a high refractive index or to provide the high refractive index coatings in optical stacks.
  • the existing process for producing titanium dioxide coatings comprises using titanium metal as the sputtering target and using oxygen as a component of the plasma gas. The titanium is thus converted to titanium dioxide during the sputtering process. Although satisfactory coatings of titanium dioxide can be produced, the rate of production is very slow and much slower than coating with silica.
  • niobium oxide As a substitute for titanium dioxide it has been suggested to use alternative materials such as niobium oxide. Whilst it is possible to coat a substrate with niobium oxide using a niobium metal target at slightly higher speeds than the equivalent process using titanium, niobium is very expensive.
  • titanium dioxide can be sputtered from a target comprising sub-stoichiometric titanium dioxide to provide coatings on a substrate either of sub-stoichiometric titanium dioxide, or titanium dioxide, depending upon the sputtering conditions.
  • the present invention provides a sputtering target which comprises sub-stoichiometric titanium dioxide, TiO x , where x is below 2.
  • Sub-stoichiometric titanium dioxide, TiO x , where x is below 2 and generally is in the range of from 1.55 to 1.95 is known in the art. It may be produced by the reduction of stoichiometric TiO 2 . It is a form of titanium dioxide which is conductive.
  • the sputtering target of the present invention may comprise sub-stoichiometric titanium dioxide, TiO x coated onto a target base.
  • a target base such as a backing tube or plate, for example a target base of an electrically conductive material, for example stainless steel or titanium metal.
  • the target may be of any type known in the art, for example a rotatable target or a flat magnetron target.
  • the sputtering target of the present invention may be prepared by plasma spraying titanium dioxide onto a target base. During the plasma spraying process, the titanium dioxide loses some oxygen atoms from its lattice and is converted into the sub-stoichiometric form.
  • the primary plasma gas used for the plasma spraying is preferably argon, with hydrogen as the secondary plasma gas.
  • the titanium dioxide which is subjected to plasma spraying preferably has a particle size in the range of from 1 to 60 micrometers. It is also important to cool the sputtering target during the plasma spraying in order to quench the titanium dioxide in sub-stoichiometric form and to improve the conductivity thereof. It also important to use a certain amount of hydrogen in the plasma gas in order to produce a high temperature plasma and to assist in the reduction.
  • the present invention also provides in another aspect a process for coating a substrate surface with titanium dioxide, which process comprises using as a sputtering target a target comprising sub-stoichiometric titanium dioxide, TiO x .
  • the sputtering from the target is preferably carried out using as the plasma gas argon, a mixture of argon and oxygen, a mixture of nitrogen and argon, or a mixture of nitrogen and oxygen. If the plasma gas does not contain oxygen, e.g. if pure argon is used, then the coating will comprise sub-stoichiometric titanium dioxide.
  • the coating is not completely transparent and possesses some conductivity.
  • the sub-stoichiometric form of titanium dioxide is converted into the transparent form which is stoichiometric or substantially stoichiometric.
  • the degree of transparency will depend upon the amount of oxygen contained in the plasma gas.
  • a preferred gas mixture to form transparent titanium dioxide as the coating comprises 70-90% by volume argon and 30-10% by volume of oxygen.
  • the substrate which is coated according to this process may comprise, for example, optical glass, the screen of a cathode ray tube, such as a TV screen, cold mirrors, low-emissivity glasses, architectural glasses, antireflective panels, flexible films or oxygen barrier films.
  • the coating process will be carried out under conditions such that the sub-stoichiometric titanium dioxide is converted into the stoichiometric form.
  • the present invention also provides a process for the preparation of sub-stoichiometric titanium dioxide, TiO x , where x is below 2 which process comprises subjecting titanium dioxide to a plasma flame.
  • the titanium dioxide is preferably sprayed through a plasma flame, for example a plasma flame using a mixture of argon and hydrogen as the plasma gas.
  • the main advantage of the present invention is that from the sub-stoichiometric titanium dioxide targets used in the present invention the rate of sputtering is increased by a factor of about ten as compared to sputtering from a titanium metal target, thus making the process industrially attractive.
  • a rotatable target comprising a tube of titanium metal of diameter 133 mm and length 800 mm was used to sputter titanium metal onto a glass plate placed at a distance of 18 cm from the target.
  • the sputtering was carried out at a power level of 35 kW (80A, 446V) under a pressure of 5 ⁇ 10 ⁇ 3 mBar of argon as the plasma gas.
  • Example 1 The procedure of Example 1 was repeated but substituting a mixture of 80% O 2 and 20% Ar as the primary plasma gas to replace the argon primary plasma gas of Example 1.
  • the sputtering was carried out at a power level of 45 kW (97A, 460V) under a pressure of 4.5 ⁇ 10 ⁇ 3 mBar.
  • a titanium metal target as described in Example 1 a titanium dioxide layer of thickness 1500 Angstroms was deposited on a glass plate place above the target in 31 ⁇ 2 minutes.
  • a rotatable target comprising a tube of stainless steel of diameter 133 mm and length 800 mm was coated with sub-stoichiometric titanium dioxide, TiO x , where x is below 2 as hereinbefore described by plasma spraying titanium dioxide onto the target using argon as the primary plasma gas and hydrogen as the secondary plasma gas. 72 liters (60% argon, 40% hydrogen) were used. The power level was 45 kW (455A, 96V).
  • This target was then used as a sputtering target in the manner as described in Example 1.
  • argon as the primary plasma gas the sputtering was carried out at a power level of 45 kW (97A, 460V) under a pressure of 5.4 ⁇ 10 ⁇ 3 mBar Ar.
  • a rotatable target prepared as described in Example 3 was used as a sputtering target in the manner as described in Example 3 using a mixture of 75% Ar and 25% O 2 as the plasma gas.
  • the sputtering was carried out at a power of 45 kW (95A, 473V) under a pressure of 5 ⁇ 10 ⁇ 3 mBar.
  • a clear transparent coating of stoichiometric titanium dioxide of thickness 12500 Angstroms was deposited on a glass plate placed above the target in 31 ⁇ 2 minutes. The sputtering proceeded smoothly without significant arcing.
  • a rotatable target was prepared as described in Example 3 by using pure argon (40 liters) at a power level of 34 kW (820A, 42V).
  • the electrical conductivity of the target was ten times inferior to that of Example 3. Sputtering from the target was difficult due to arcing. The process was not stable enough to produce samples.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Plasma & Fusion (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Physical Vapour Deposition (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Coating By Spraying Or Casting (AREA)
  • Surface Treatment Of Glass (AREA)
  • Surface Treatment Of Optical Elements (AREA)
  • Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)

Abstract

Sputtering targets comprising sub-stoichiometric titanium dioxide, TiOx, where x is below 2, are provided. The targets are preferably formed by plasma spraying so as to have an electrical resistivity of less than 0.5 ohm.cm.

Description

  • The present invention relates to improved sputtering targets and, in particular to sputtering targets of titanium dioxide, and to a method for the preparation thereof. [0001]
  • Sputtered coatings of various oxides (e.g. silica) and nitrides (e.g. silicon nitride) are used to form optical coatings showing interesting properties on a number of substrates. Known applications include low emissivity films on window glasses, cold mirrors on reflectors, enhanced mirrors for photocopiers and antireflective coatings on picture glass or TV screens. These coatings are usually made of stacks of several different layers with different refractive indices, preferably of low and high refractive index, to produce optical filters. For antireflective coatings it is preferred to combine two materials showing the highest and the lowest possible refractive indices. Such materials are titania and silica. Another advantage of these materials is their durability. [0002]
  • Titanium dioxide coatings have a high refractive index and can thus be used to provide coatings of a high refractive index or to provide the high refractive index coatings in optical stacks. The existing process for producing titanium dioxide coatings comprises using titanium metal as the sputtering target and using oxygen as a component of the plasma gas. The titanium is thus converted to titanium dioxide during the sputtering process. Although satisfactory coatings of titanium dioxide can be produced, the rate of production is very slow and much slower than coating with silica. [0003]
  • As a substitute for titanium dioxide it has been suggested to use alternative materials such as niobium oxide. Whilst it is possible to coat a substrate with niobium oxide using a niobium metal target at slightly higher speeds than the equivalent process using titanium, niobium is very expensive. [0004]
  • Thus, there is a need for an improved process for coating titanium dioxide onto substrate materials. We have now surprisingly discovered that titanium dioxide can be sputtered from a target comprising sub-stoichiometric titanium dioxide to provide coatings on a substrate either of sub-stoichiometric titanium dioxide, or titanium dioxide, depending upon the sputtering conditions. [0005]
  • Accordingly, the present invention provides a sputtering target which comprises sub-stoichiometric titanium dioxide, TiO[0006] x, where x is below 2. Sub-stoichiometric titanium dioxide, TiOx, where x is below 2 and generally is in the range of from 1.55 to 1.95 is known in the art. It may be produced by the reduction of stoichiometric TiO2. It is a form of titanium dioxide which is conductive.
  • The sputtering target of the present invention may comprise sub-stoichiometric titanium dioxide, TiO[0007] x coated onto a target base. such as a backing tube or plate, for example a target base of an electrically conductive material, for example stainless steel or titanium metal. The target may be of any type known in the art, for example a rotatable target or a flat magnetron target.
  • The sputtering target of the present invention may be prepared by plasma spraying titanium dioxide onto a target base. During the plasma spraying process, the titanium dioxide loses some oxygen atoms from its lattice and is converted into the sub-stoichiometric form. The primary plasma gas used for the plasma spraying is preferably argon, with hydrogen as the secondary plasma gas. The titanium dioxide which is subjected to plasma spraying preferably has a particle size in the range of from 1 to 60 micrometers. It is also important to cool the sputtering target during the plasma spraying in order to quench the titanium dioxide in sub-stoichiometric form and to improve the conductivity thereof. It also important to use a certain amount of hydrogen in the plasma gas in order to produce a high temperature plasma and to assist in the reduction. [0008]
  • The present invention also provides in another aspect a process for coating a substrate surface with titanium dioxide, which process comprises using as a sputtering target a target comprising sub-stoichiometric titanium dioxide, TiO[0009] x. The sputtering from the target is preferably carried out using as the plasma gas argon, a mixture of argon and oxygen, a mixture of nitrogen and argon, or a mixture of nitrogen and oxygen. If the plasma gas does not contain oxygen, e.g. if pure argon is used, then the coating will comprise sub-stoichiometric titanium dioxide. The coating is not completely transparent and possesses some conductivity. If, however, the plasma gas contains oxygen then the sub-stoichiometric form of titanium dioxide is converted into the transparent form which is stoichiometric or substantially stoichiometric. The degree of transparency will depend upon the amount of oxygen contained in the plasma gas. A preferred gas mixture to form transparent titanium dioxide as the coating comprises 70-90% by volume argon and 30-10% by volume of oxygen.
  • The substrate which is coated according to this process may comprise, for example, optical glass, the screen of a cathode ray tube, such as a TV screen, cold mirrors, low-emissivity glasses, architectural glasses, antireflective panels, flexible films or oxygen barrier films. In this case the coating process will be carried out under conditions such that the sub-stoichiometric titanium dioxide is converted into the stoichiometric form. [0010]
  • In a further aspect the present invention also provides a process for the preparation of sub-stoichiometric titanium dioxide, TiO[0011] x, where x is below 2 which process comprises subjecting titanium dioxide to a plasma flame. In carrying out this process the titanium dioxide is preferably sprayed through a plasma flame, for example a plasma flame using a mixture of argon and hydrogen as the plasma gas.
  • The main advantage of the present invention is that from the sub-stoichiometric titanium dioxide targets used in the present invention the rate of sputtering is increased by a factor of about ten as compared to sputtering from a titanium metal target, thus making the process industrially attractive. [0012]
  • The present invention will be further described with reference to the following Examples.[0013]
    • EXAMPLE 1 Comparative
  • A rotatable target comprising a tube of titanium metal of diameter 133 mm and length 800 mm was used to sputter titanium metal onto a glass plate placed at a distance of 18 cm from the target. The sputtering was carried out at a power level of 35 kW (80A, 446V) under a pressure of 5×10[0014] −3 mBar of argon as the plasma gas.
  • After 3½ minutes a layer of titanium metal 18000 Angstroms in thickness as measured by a profilometer had been deposited upon the glass plate. [0015]
    • EXAMPLE 2 Comparative
  • The procedure of Example 1 was repeated but substituting a mixture of 80% O[0016] 2 and 20% Ar as the primary plasma gas to replace the argon primary plasma gas of Example 1. The sputtering was carried out at a power level of 45 kW (97A, 460V) under a pressure of 4.5×10−3 mBar. Using a titanium metal target as described in Example 1 a titanium dioxide layer of thickness 1500 Angstroms was deposited on a glass plate place above the target in 3½ minutes.
    • EXAMPLE 3
  • A rotatable target comprising a tube of stainless steel of diameter 133 mm and length 800 mm was coated with sub-stoichiometric titanium dioxide, TiO[0017] x, where x is below 2 as hereinbefore described by plasma spraying titanium dioxide onto the target using argon as the primary plasma gas and hydrogen as the secondary plasma gas. 72 liters (60% argon, 40% hydrogen) were used. The power level was 45 kW (455A, 96V).
  • This target was then used as a sputtering target in the manner as described in Example 1. Using argon as the primary plasma gas the sputtering was carried out at a power level of 45 kW (97A, 460V) under a pressure of 5.4×10[0018] −3 mBar Ar. A dark blue semitransparent layer of sub-stoichiometric titanium dioxide, TiOx, of thickness 14000 Angstroms was deposited on a glass plate placed above the target in 3½ minutes. The sputtering proceeded smoothly without significant arcing.
    • EXAMPLE 4
  • A rotatable target prepared as described in Example [0019] 3 was used as a sputtering target in the manner as described in Example 3 using a mixture of 75% Ar and 25% O2 as the plasma gas. The sputtering was carried out at a power of 45 kW (95A, 473V) under a pressure of 5×10−3 mBar. A clear transparent coating of stoichiometric titanium dioxide of thickness 12500 Angstroms was deposited on a glass plate placed above the target in 3½ minutes. The sputtering proceeded smoothly without significant arcing.
    • EXAMPLE 5 Comparative
  • A rotatable target was prepared as described in Example 3 by using pure argon (40 liters) at a power level of 34 kW (820A, 42V). The electrical conductivity of the target was ten times inferior to that of Example 3. Sputtering from the target was difficult due to arcing. The process was not stable enough to produce samples. [0020]

Claims (15)

1. A sputtering target which comprises sub-stoichiometric titanium dioxide, TiOx, where x is below 2.
2. A sputtering target as claimed in claim 1 wherein the TiOx is coated onto an electrically conductive base.
3. A process for the preparation of a sputtering target as claimed in claim 1 or claim 2, which process comprises plasma spraying titanium dioxide, TiO2, onto a target base.
4. A process as claimed in claim 3 wherein the target base is cooled during the plasma spraying.
5. A process as claimed in claim 3 or claim 4 wherein the plasma spraying is carried out using argon as the plasma gas and hydrogen as the secondary plasma gas.
6. A process as claimed in any one of claims 3 to 5 wherein the target bas e is titanium.
7. A process as claimed in any one of claims 3 to 6 wherein the titanium dioxide which is plasma sprayed has particle size in the range of from 1 to 60 micrometers.
8. A process for coating a substrate surface with titanium dioxide, which process comprises the use as a sputtering target of a target as claimed in claim 1 or claim 2.
9. A process as claimed in claim 8 wherein the sputtering from the target is carried out using as the plasma gas argon, a mixture of argon and oxygen, a mixture or argon and nitrogen, or a mixture of nitrogen and oxygen.
10. A process as claimed in claim 9 wherein the plasma gas comprises 70 to 90% by volume argon and 30 to 10% by volume oxygen.
11. A process as claimed in any one of claims 8 to 10 wherein the substrate which is coated is optical glass, the screen of a cathode ray tube, a flexible film or an oxygen barrier film.
12. A substrate which has been coated by a process as claimed in any one of claims 8 to 11.
13. A process for the preparation of sub-stoichiometric titanium dioxide, TiOx, where x is below 2 which process comprises subjecting titanium dioxide to a plasma flame.
14. A process as claimed in claim 13 wherein titanium dioxide is sprayed through a plasma flame.
15. A process as claimed in claim 13 wherein the titanium dioxide is sprayed using a combustion flame.
US09/966,636 1996-01-05 2001-09-28 Sputtering targets and method for the preparation thereof Abandoned US20020081465A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US09/966,636 US20020081465A1 (en) 1996-01-05 2001-09-28 Sputtering targets and method for the preparation thereof

Applications Claiming Priority (8)

Application Number Priority Date Filing Date Title
GBGB9600210.0A GB9600210D0 (en) 1996-01-05 1996-01-05 Improved sputtering targets and method for the preparation thereof
GB9600210.0 1996-01-05
EPPCT/EP97/00020 1997-01-03
PCT/EP1997/000021 WO1997025450A1 (en) 1996-01-05 1997-01-03 Process for coating a substrate with titanium dioxide
PCT/EP1997/000020 WO1997025451A1 (en) 1996-01-05 1997-01-03 Sputtering targets and method for the preparation thereof
EPPCT/EP97/00021 1997-01-03
US4468198A 1998-03-06 1998-03-06
US09/966,636 US20020081465A1 (en) 1996-01-05 2001-09-28 Sputtering targets and method for the preparation thereof

Related Parent Applications (1)

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US4468198A Continuation 1996-01-05 1998-03-06

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US20020081465A1 true US20020081465A1 (en) 2002-06-27

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US09/101,405 Expired - Lifetime US6461686B1 (en) 1996-01-05 1997-01-03 Sputtering targets and method for the preparation thereof
US09/589,098 Expired - Fee Related US6468402B1 (en) 1996-01-05 2000-06-08 Process for coating a substrate with titanium dioxide
US09/759,661 Abandoned US20010019738A1 (en) 1996-01-05 2001-01-12 Sputtering targets and method for the preparation thereof
US09/780,537 Abandoned US20010010288A1 (en) 1996-01-05 2001-02-12 Sputtering targets and method for the preparation thereof
US09/899,581 Abandoned US20020071971A1 (en) 1996-01-05 2001-07-05 Process for coating a substrate with titanium dioxide
US09/966,636 Abandoned US20020081465A1 (en) 1996-01-05 2001-09-28 Sputtering targets and method for the preparation thereof
US10/032,901 Abandoned US20020127349A1 (en) 1996-01-05 2001-10-19 Sputtering targets and method for the preparation thereof
US10/001,964 Expired - Fee Related US6511587B2 (en) 1996-01-05 2001-12-05 Sputtering targets and method for the preparation thereof
US10/008,949 Abandoned US20020125129A1 (en) 1996-01-05 2001-12-07 Sputtering targets and method for the preparation thereof
US10/417,413 Abandoned US20040069623A1 (en) 1996-01-05 2003-04-17 Sputtering targets and method for the preparation thereof
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US09/759,661 Abandoned US20010019738A1 (en) 1996-01-05 2001-01-12 Sputtering targets and method for the preparation thereof
US09/780,537 Abandoned US20010010288A1 (en) 1996-01-05 2001-02-12 Sputtering targets and method for the preparation thereof
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US10/008,949 Abandoned US20020125129A1 (en) 1996-01-05 2001-12-07 Sputtering targets and method for the preparation thereof
US10/417,413 Abandoned US20040069623A1 (en) 1996-01-05 2003-04-17 Sputtering targets and method for the preparation thereof
US11/346,372 Abandoned US20060249373A1 (en) 1996-01-05 2006-02-03 Sputtering targets and method for the preparation thereof

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EP0871794B1 (en) 2002-09-18
DE69723053D1 (en) 2003-07-31
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CN1208495C (en) 2005-06-29
DE69723053T2 (en) 2004-05-19
US20010019738A1 (en) 2001-09-06
KR100510609B1 (en) 2005-10-25
US6511587B2 (en) 2003-01-28
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CA2241878C (en) 2009-07-21
US20020127349A1 (en) 2002-09-12
EP0871792A1 (en) 1998-10-21
CN1212026A (en) 1999-03-24
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JP4087447B2 (en) 2008-05-21
US20020071971A1 (en) 2002-06-13
US20010010288A1 (en) 2001-08-02
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US6468402B1 (en) 2002-10-22
AU1439097A (en) 1997-08-01
GB9600210D0 (en) 1996-03-06
US20020125129A1 (en) 2002-09-12
IL125103A0 (en) 1999-01-26
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US20040069623A1 (en) 2004-04-15
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US20060249373A1 (en) 2006-11-09
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