Patents by Inventor Hidekimi Kadokura

Hidekimi Kadokura has filed for patents to protect the following inventions. This listing includes patent applications that are pending as well as patents that have already been granted by the United States Patent and Trademark Office (USPTO).

  • Patent number: 8293327
    Abstract: The present invention provides a process for forming a strontium-containing thin film of a cyclopentadienyl-based strontium compound, which is in the liquid state at room temperature to 50° C., can be purified by distillation, present as a monomer, has high vapor pressure, and suitable for mass production. bis(propyltetramethylcyclopentadienyl)strontium is used as an Sr source to form a strontium-containing thin film such as a SrTiO3 film, a (Ba, Sr)TiO3 film by chemical vapor deposition or atomic layer deposition.
    Type: Grant
    Filed: June 25, 2008
    Date of Patent: October 23, 2012
    Assignees: Kabushikikaisha Kojundokagaku Kenkyusho, Tokyo Electron Limited
    Inventors: Hidekimi Kadokura, Shintaro Higashi, Yoshinori Kuboshima, Yumiko Kawano
  • Patent number: 7816282
    Abstract: A method is used for forming an SrTiO3 film on a substrate placed and heated inside a process chamber while supplying a gaseous Ti source material, a gaseous Sr source material, and a gaseous oxidizing agent into the process chamber. Sr(C5(CH3)5)2 is used as the Sr source material. The method performs a plurality of cycles to form the SrTiO3 film. Each cycle sequentially includes supplying the gaseous Ti source material into the process chamber and thereby adsorbing it onto the substrate; supplying the gaseous oxidizing agent into the process chamber and thereby decomposing the Ti source material thus adsorbed and forming a Ti-containing oxide film; supplying the gaseous Sr source material into the process chamber and thereby adsorbing it onto the Ti-containing oxide film; and supplying the gaseous oxidizing agent into the process chamber and thereby decomposing the Sr source material thus adsorbed and forming an Sr-containing oxide film.
    Type: Grant
    Filed: January 24, 2008
    Date of Patent: October 19, 2010
    Assignee: Tokyo Electron Limited
    Inventors: Yumiko Kawano, Akinobu Kakimoto, Hidekimi Kadokura, Shintaro Higashi
  • Patent number: 7635441
    Abstract: The present invention provides a raw material for forming a strontium-containing thin film of a cyclopentadienyl-based strontium compound, which is in the liquid state at room temperature to 50° C., can be purified by distillation, present as a monomer, has high vapor pressure, and suitable for mass production, and a process for preparing the same. Sr[C5(CH3)4(C3H7)]2 is prepared by reacting Na[C5(CH3)4(C3H7)]2 or K[C5(CH3)4(C3H7)]2 with SrI2 in THF to produce a THF adduct of Sr[C5(CH3)4(C3H7)]2; evaporating THF and extracting the residue with toluene to give a toluene solution; evaporating toluene and drying the residue under reduced pressure; and heating to 100 to 160° C. in vacuo to dissociate and remove THF and distilling.
    Type: Grant
    Filed: June 25, 2008
    Date of Patent: December 22, 2009
    Assignee: Kabushikikaisha Kojundokagaku Kenkyusho
    Inventors: Hidekimi Kadokura, Shintaro Higashi, Yoshinori Kuboshima
  • Publication number: 20090001618
    Abstract: The present invention provides a raw material for forming a strontium-containing thin film of a cyclopentadienyl-based strontium compound, which is in the liquid state at room temperature to 50° C., can be purified by distillation, present as a monomer, has high vapor pressure, and suitable for mass production, and a process for preparing the same. Sr[C5(CH3)4(C3H7)]2 is prepared by reacting Na[C5(CH3)4(C3H7)]2 or K[C5(CH3)4(C3H7)]2 with SrI2 in THF to produce a THF adduct of Sr[C5(CH3)4(C3H7)]2; evaporating THF and extracting the residue with toluene to give a toluene solution; evaporating toluene and drying the residue under reduced pressure; and heating to 100 to 160° C. in vacuo to dissociate and remove THF and distilling.
    Type: Application
    Filed: June 25, 2008
    Publication date: January 1, 2009
    Applicant: Kabushikikaisha Kojundokagaku Kenkyusho
    Inventors: Hidekimi KADOKURA, Shintaro HIGASHI, Yoshinori KUBOSHIMA
  • Publication number: 20090004383
    Abstract: The present invention provides a process for forming a strontium-containing thin film of a cyclopentadienyl-based strontium compound, which is in the liquid state at room temperature to 50° C., can be purified by distillation, present as a monomer, has high vapor pressure, and suitable for mass production. bis(propyltetramethylcyclopentadienyl)strontium is used as an Sr source to form a strontium-containing thin film such as a SrTiO3 film, a (Ba, Sr)TiO3 film by chemical vapor deposition or atomic layer deposition.
    Type: Application
    Filed: June 25, 2008
    Publication date: January 1, 2009
    Applicants: KABUSHIKIKAISHA KOJUNDOKAGAKU KENKYUSHO, TOKYO ELECTRON LIMITED
    Inventors: Hidekimi KADOKURA, Shintaro HIGASHI, Yoshinori KUBOSHIMA, Yumiko KAWANO
  • Publication number: 20080175994
    Abstract: A method is used for forming an SrTiO3 film on a substrate placed and heated inside a process chamber while supplying a gaseous Ti source material, a gaseous Sr source material, and a gaseous oxidizing agent into the process chamber. Sr(C5(CH3)5)2 is used as the Sr source material. The method performs a plurality of cycles to form the SrTiO3 film. Each cycle sequentially includes supplying the gaseous Ti source material into the process chamber and thereby adsorbing it onto the substrate; supplying the gaseous oxidizing agent into the process chamber and thereby decomposing the Ti source material thus adsorbed and forming a Ti-containing oxide film; supplying the gaseous Sr source material into the process chamber and thereby adsorbing it onto the Ti-containing oxide film; and supplying the gaseous oxidizing agent into the process chamber and thereby decomposing the Sr source material thus adsorbed and forming an Sr-containing oxide film.
    Type: Application
    Filed: January 24, 2008
    Publication date: July 24, 2008
    Applicant: TOKYO ELECTRON LIMITED
    Inventors: Yumiko KAWANO, Akinobu Kakimoto, Hidekimi Kadokura, Shintaro Higashi
  • Patent number: 6930177
    Abstract: The invention provides true La(OiPr)3 preferable as a starting material for an asymmetric synthesis catalyst and a process for producing the same. In this process, anhydrous lanthanum chloride LaCl3 is reacted with potassium isopropoxide K(OiPr) in a mixed solvent of isopropanol and toluene, then the isopropanol is distilled away to replace all the solvent by toluene, then the reaction solution is left, decanted and filtered to give a transparent filtrate, and the solvent is distilled away from the filtrate which is then vacuum-dried under heating, whereby high-purity La(OiPr)3 is obtained in 77% yield. In this high-purity La(OiPr)3, the La content is 97 to 103% of the theoretical content, impurity K is 0.3% or less, (Li+Na) is 0.01% or less, Cl is 0.2% or less, and the degree of association thereof is 5.5 to 6.5.
    Type: Grant
    Filed: August 7, 2002
    Date of Patent: August 16, 2005
    Assignee: Kabushikikaisha Kojundokagaku Kenkyusho
    Inventors: Hidekimi Kadokura, Masamichi Matsumoto, Tadashi Ishii, Yumie Okuhara, Yoshinori Kuboshima, Hiroshi Matsumoto
  • Patent number: 6872419
    Abstract: A method or process for producing PZT films by using a Ti material having a broad allowable temperature range for providing a predetermined film composition, easily thermally deposited from Ti(OiPr)2(dibm)2 at a low substrate temperature of 450° C. or less in CVD. Starting materials are fed in a solution vaporization system. The starting materials, Ti (OiPr)2(dibm)2, used as a T1 source, and a combination of Pb(dpm)2-Zr(Oipr)(dpm)3-Ti(OiPr)2(dibm)2 in n-butyl acetate are vaporized and supplied at 200° C. The vaporized starting materials are fed into a chamber and subjected to CVD at a substrate temperature of 420° C. at 1 Torr in an oxygen atmosphere, whereby excellent PZT films can be produced. Ti(OiPr)2(dibm)2 has a melting point of 105° C., a high solubility and a vapor pressure of 1 Torr/150° C. and does not react with Pb(dpm)2, and a solution thereof in n-butyl acetate has a pot life of 3 months.
    Type: Grant
    Filed: December 13, 2002
    Date of Patent: March 29, 2005
    Assignee: Kabushikikaisha Kojundokagaku Kenkyusho
    Inventors: Hidekimi Kadokura, Yumie Okuhara
  • Publication number: 20030153100
    Abstract: This invention provides a process for producing PZT films by specifying a Ti material having a broad allowable temperature range for giving a predetermined film composition, easily thermally deposited from Ti(OiPr)2(dpm)2 even at a low substrate temperature of 450° C. or less in CVD where starting materials are fed in a solution vaporization system. Ti(OiPr)2(dibm)2 is used as a Ti source, and a solution of a combination of Pb(dpm)2-Zr(OiPr)(dpm)3-Ti(OiPr)2(dibm)2 in n-butyl acetate is vaporized and supplied at 200° C., and subjected to CVD at a substrate temperature of 420° C. at 1 Torr in an oxygen atmosphere, whereby excellent PZT films can be produced.
    Type: Application
    Filed: December 13, 2002
    Publication date: August 14, 2003
    Inventors: Hidekimi Kadokura, Yumie Okuhara
  • Patent number: 6593484
    Abstract: A stable compound having a vapor pressure higher by 1 order than that of Ta(NtBu)(NEt2)3 is provided as a starting material for forming a TaN film as a barrier film by the CVD method. There are further provided a process for producing the same and a method of forming a TaN film by using the same. The novel compound, tantalum tertiary amylimido tris(dimethylamide) [Ta(NtAm)(NMe2)3] has a vapor pressure of 1 Torr at 80° C., and its melting point is 36° C. This compound is obtained by allowing 1 mole of TaCl5, 4 moles of LiNMe2 and 1 mole of LiNHtAm to react with one another in an organic solvent in the vicinity of room temperature, then separating byproducts by filtration, distilling the solvent away, and distilling the product in vacuo. This compound can be used as a starting material in CVD to form a cubic TaN film on a SiO2/Si substrate at 550° C. at 0.05 Torr.
    Type: Grant
    Filed: November 9, 2001
    Date of Patent: July 15, 2003
    Assignee: Kabushikikaisha Kojundokagaku Kenkyusho
    Inventors: Sakiko Yasuhara, Hidekimi Kadokura
  • Publication number: 20030055228
    Abstract: The invention provides true La(OiPr)3 preferable as a starting material for an asymmetric synthesis catalyst and a process for producing the same. In this process, anhydrous lanthanum chloride LaCl3 is reacted with potassium isopropoxide K(OiPr) in a mixed solvent of isopropanol and toluene, then the isopropanol is distilled away to replace all the solvent by toluene, then the reaction solution is left, decanted and filtered to give a transparent filtrate, and the solvent is distilled away from the filtrate which is then vacuum-dried under heating, whereby high-purity La(OiPr)3 is obtained in 77% yield. In this high-purity La(OiPr)3, the La content is 97 to 103% of the theoretical content, impurity K is 0.3% or less, (Li+Na) is 0.01% or less, Cl is 0.2% or less, and the degree of association thereof is 5.5 to 6.5.
    Type: Application
    Filed: August 7, 2002
    Publication date: March 20, 2003
    Inventors: Hidekimi Kadokura, Masamichi Matsumoto, Tadashi Ishii, Yumie Okuhara, Yoshinori Kuboshima, Hiroshi Matsumoto
  • Publication number: 20020169335
    Abstract: This invention provides a process for producing bismuth tertiary amyloxide which is a starting material for forming a ferroelectric film such as SrBi2Ta2O9 containing bismuth oxide, or an oxide superconductive film such as Bi2Sr2CaCu2O8, by the CVD method or sol-gel method. This process comprises reacting bismuth bromide with sodium tertiary amyloxide or potassium tertiary amyloxide in a toluene solvent containing 5 to 30 weight % tetrahydrofuran, then separating a byproduct sodium bromide or potassiumbromide by filtration and recovering bismuth tertiary amyloxide by distillation under reduced pressure.
    Type: Application
    Filed: February 20, 2002
    Publication date: November 14, 2002
    Inventors: Satoru Morisawa, Masamichi Matsumoto, Hidekimi Kadokura
  • Patent number: 6472547
    Abstract: This invention provides a process for producing bismuth tertiary amyloxide which is a starting material for forming a ferroelectric film such as SrBi2Ta2O9 containing bismuth oxide, or an oxide superconductive film such as Bi2Sr2CaCu2O8, by the CVD method or sol-gel method. This process comprises reacting bismuth bromide with sodium tertiary amyloxide or potassium tertiaryamyloxide in a toluene solvent containing 5 to 30 weight % tetrahydrofuran, then separating a byproduct sodium bromide or potassium bromide by filtration and recovering bismuth tertiary amyloxide by distillation under reduced pressure.
    Type: Grant
    Filed: February 20, 2002
    Date of Patent: October 29, 2002
    Assignee: Kabushikikaisha Kojundokagaku Kenyusho
    Inventors: Satoru Morisawa, Masamichi Matsumoto, Hidekimi Kadokura
  • Patent number: 6469189
    Abstract: A novel compound shown by M[N(OC2H5)5(OC2H4OCH3)]2, wherein M represents Sr or Ba, N represents Nb or Ta, which is a liquid at room temperature, is hard to be thermally dissociated, and has a vapor pressure of about 0.2 Torr at 190° C. The compound is produced by reacting 2 moles of N(OC2H5)5 and from 1 to 1.1 moles of M(OC2H4OCH3)2 and then recovering the product by distillation. By using the compounds as raw materials for a CVD method, an SrBi2Ta2O9 thin film or a (Sr0.75Ba0.25)Nb2O6 thin film for semiconductor devices can be produced.
    Type: Grant
    Filed: February 17, 2000
    Date of Patent: October 22, 2002
    Assignee: Kabushikikaisha Kojundokagaku Kenkyusho
    Inventors: Hidekimi Kadokura, Yumie Okuhara
  • Publication number: 20020115886
    Abstract: A stable compound having a vapor pressure higher by 1 order than that of Ta(NtBu)(NEt2)3 is provided as a starting material for forming a TaN film as a barrier film by the CVD method. There are further provided a process for producing the same and a method of forming a TaN film by using the same. The novel compound, tantalum tertiary amylimido tris(dimethylamide) [Ta(NtAm)(NMe2)3] has a vapor pressure of 1 Torr at 80 ° C., and its melting point is 36° C. This compound is obtained by allowing 1 mole of TaCl5, 4 moles of LiNMe2 and 1 mole of LiNHtAm to react with one another in an organic solvent in the vicinity of room temperature, then separating byproducts by filtration, distilling the solvent away, and distilling the product in vacuo. This compound can be used as a starting material in CVD to form a cubic TaN film on a SiO2/Si substrate at 550° C. at 0.05 Torr.
    Type: Application
    Filed: November 9, 2001
    Publication date: August 22, 2002
    Inventors: Sakiko Yasuhara, Hidekimi Kadokura
  • Patent number: 6426425
    Abstract: The invention provides a process for purifying gallium alkoxides by decreasing the amount of impurity chlorine contained therein, gallium alkoxides which are useful as raw materials for the formation of dielectrics containing gallium oxide and as raw materials for the syntheses of compounds for photoelectronics. Gallium isopropoxide containing 0.98 weight percent of chlorine and potassium isopropoxide of 1.4 equivalents to the impurity chlorine are refluxed in toluene as a solvent for 5 hours, the solvent is distilled away, and the residue is simply distilled under vacuum to obtain gallium isopropoxide containing 0.022 weight percent of the chlorine in a 89% yield.
    Type: Grant
    Filed: March 2, 2001
    Date of Patent: July 30, 2002
    Assignee: Kabushikikaisha Kojundokagaku Kenkyusho
    Inventors: Hidekimi Kadokura, Tadashi Ishii
  • Patent number: 6376692
    Abstract: There is provided a compound for the formation of a PZT film using Pb(dpm)2 where the compound has a low reactivity with Pb(dpm)2, has a thermal decomposition temperature which is lower than Zr(dpm)4 and is well soluble in a solvent such as butyl acetate and toluene. There is also provided a process for the manufacture of the compound. There is further provided a liquid composition for the formation of a PZT film using the compound. The novel compound Zr(OiPr)(dpm)3 has a sublimation pressure of 0.1 Torr/160° C. and is able to form a ZrO2 film by a CVD at 400° C. That can be prepared by the reaction of 1 mol of Zr(OiPr)4 and 3 mol of dpmH in an organic solvent followed by purifying by sublimation. A solution of Pb(dpm)2, Zr(OiPr)(dpm)3 and Ti(OiPr)2(dpm)2 dissolved in butyl acetate has a long pot life and forms a PZT film by a solution flash CVD method.
    Type: Grant
    Filed: October 5, 2000
    Date of Patent: April 23, 2002
    Assignee: Kabushikikaisha Kojundokagaku Kenkyusho
    Inventors: Hidekimi Kadokura, Yumie Okuhara
  • Patent number: 6207232
    Abstract: To provide Ru compounds which are in the form of a liquid at room temperature to be used in forming Ru and RuO2 films for electrodes in semiconductor devices by the CVD method and a process for producing these compounds. Because of being a liquid at room temperature and having a sufficient vapor ressure at about 100° C., bis(ethylcyclopentadienyl)ruthenium or bis(isopropylcyclopentadienyl)ruthenium can be quantitatively supplied via gas bubbling or with the use of a liquid mass flow controller as a feedstock in the CVD method and thermally decomposed on a substrate at 600° C. in a hydrogen atmosphere to give pure Ru films. These compounds can be obtained at a high yield by reacting respectively ruthenium trichloride hydrate and ethylcyclopentadiene or isopropylcyclopentadiene with a zinc powder in an alcohol solvent at −30 to 0° C.
    Type: Grant
    Filed: June 15, 1998
    Date of Patent: March 27, 2001
    Assignee: Kabushikikaisha Kojundokagaku Kenkyusho
    Inventor: Hidekimi Kadokura
  • Patent number: 6046345
    Abstract: Novel one-source compounds for producing (Ba,Sr)TiO.sub.3 films having high dielectric constants and ferroelectric (Sr,Ba)Nb.sub.2 O.sub.6 films by the CVD method, which are in the form of a liquid at the source temperature and contain Ba and Sr at a specified ratio; processes for producing these novel compounds; and processes for producing films by using the same.Because of having a melting point of 160.degree. C., being in the form of a liquid and having enough vapor pressure at 200.degree. C., the novel compounds barium strontium .beta.-diketonate [Ba.sub.2 Sr(dpm).sub.6 and BaSr.sub.2 (dpm).sub.6 ] can be quantitatively supplied by gas bubbling as a feedstock in the CVD method while maintaining the Ba/Sr ratio at a constant ratio. Thus, barium strontium-containing oxide dielectric films can be produced at a high reproducibility by thermal decomposition on a substrate in an oxidative atmosphere. These compounds can be produced by reacting dpmh with Ba and Sr, Ba(dpm).sub.2 with Sr(dpm).sub.
    Type: Grant
    Filed: February 17, 1999
    Date of Patent: April 4, 2000
    Assignee: Kabushikikaisha Kojundokagaku Kenkyusho
    Inventors: Hidekimi Kadokura, Yumie Okuhara
  • Patent number: 6002036
    Abstract: To provide Ru compounds which are in the form of a liquid at room temperature to be used in forming Ru and RuO.sub.2 films for electrodes in semiconductor devices by the CVD method and a process for producing these compounds.Because of being a liquid at room temperature and having a sufficient vapor ressure at about 100.degree. C., bis(ethylcyclopentadienyl)ruthenium or bis(isopropylcyclopentadienyl)ruthenium can be quantitatively supplied via gas bubbling or with the use of a liquid mass flow controller as a feedstock in the CVD method and thermally decomposed on a substrate at 600.degree. C. in a hydrogen atmosphere to give pure Ru films. These compounds can be obtained at a high yield by reacting respectively ruthenium trichloride hydrate and ethylcyclopentadiene or isopropylcyclopentadiene with a zinc powder in an alcohol solvent at -30 to 0.degree. C.
    Type: Grant
    Filed: March 8, 1999
    Date of Patent: December 14, 1999
    Assignee: Kabushikikaisha Kojundokagaku Kenkyusho
    Inventor: Hidekimi Kadokura