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    Source reagent liquid delivery apparatus, and chemical vapor deposition system comprising same
    1.
    发明授权
    Source reagent liquid delivery apparatus, and chemical vapor deposition system comprising same 失效
    源试剂液体输送装置和包含该源试剂液体输送装置的化学气相沉积系统

    公开(公告)号：US5711816A

    公开(公告)日：1998-01-27

    申请号：US484025

    申请日：1995-06-07

    申请人： Peter S. Kirlin ,  Robin L. Binder ,  Robin A. Gardiner ,  Peter Van Buskirk ,  Gregory Stauf ,  Jiming Zhang

    发明人： Peter S. Kirlin ,  Robin L. Binder ,  Robin A. Gardiner ,  Peter Van Buskirk ,  Gregory Stauf ,  Jiming Zhang

    IPC分类号： C23C16/18 ,  C23C16/40 ,  C23C16/448 ,  H01L39/24 ,  C23C16/00

    CPC分类号： C23C16/4483 ,  C23C16/18 ,  C23C16/40 ,  C23C16/408 ,  C23C16/409 ,  C23C16/4481 ,  C23C16/45561 ,  H01L39/2441 ,  Y10S261/65

    摘要： A process and apparatus for delivering an involatile reagent in gaseous form, wherein an involatile reagent source liquid is flash vaporized on a vaporization matrix structure at elevated temperature. A carrier gas may be flowed past the flash vaporization matrix structure to yield a carrier gas mixture containing the flash vaporized source reagent. The matrix structure preferably has a high surface-to-volume ratio, and may suitably comprise a foraminous matrix element such as screen mesh onto which the reagent source liquid is distributed for flash vaporization. The invention is particularly useful for delivery of Group II reagents and compounds and complexes of early transition metals such as zirconium and hafnium, and may be usefully employed with Group II beta-diketonate source layers, e.g., of YBaCuO, BiSrCaCuO, and TlBaCaCuO types, as well as for forming interlayers of Group II metal fluorides between superconductor or gallium arsenide overlayers, and for depositing thin films of photonic and ferroelectric materials, e.g., BaTiO.sub.3, Ba.sub.x Sr.sub.1-x Nb.sub.2 O.sub.6, and PbZr.sub.1-x Ti.sub.x O.sub.3.

    摘要翻译： 一种用于递送气态非挥发性试剂的方法和装置，其中非挥发性试剂源液体在升高的温度下在汽化基质结构上闪蒸。 载气可以流过闪蒸基质结构以产生含有闪蒸的源试剂的载气混合物。 基体结构优选具有高的表面体积比，并且可以适当地包括诸如筛网的多孔基质元素，其上分配有试剂源液体用于闪蒸。 本发明特别可用于递送II族试剂和早期过渡金属如锆和铪的化合物和络合物，并且可以有用地用于IIB型β-二酮源层，例如YBaCuO，BiSrCaCuO和TlBaCaCuO类型， 以及用于在超导体或砷化镓覆盖层之间形成第II族金属氟化物的夹层，以及用于沉积光致电子和铁电材料的薄膜，例如BaTiO3，BaxSr1-xNb2O6和PbZr1-xTixO3。

    Apparatus and method for delivering reagents in vapor form to a CVD reactor, incorporating a cleaning subsystem
    2.
    发明授权
    Apparatus and method for delivering reagents in vapor form to a CVD reactor, incorporating a cleaning subsystem 失效
    将蒸气形式的试剂输送到包含清洁子系统的CVD反应器的装置和方法

    公开(公告)号：US5362328A

    公开(公告)日：1994-11-08

    申请号：US178933

    申请日：1994-01-07

    申请人： Robin A. Gardiner ,  Peter Van Buskirk ,  Peter S. Kirlin

    发明人： Robin A. Gardiner ,  Peter Van Buskirk ,  Peter S. Kirlin

    IPC分类号： C23C16/18 ,  C23C16/40 ,  C23C16/448 ,  H01L39/24 ,  C23C16/00

    CPC分类号： C23C16/4483 ,  C23C16/18 ,  C23C16/40 ,  C23C16/408 ,  C23C16/409 ,  C23C16/4481 ,  C23C16/45561 ,  H01L39/2441 ,  Y10S261/65 ,  Y10S261/88

    摘要： A means and method for protecting a source reagent vaporizer structure from the harmful effects of solid build-up occurring during its use in chemical vapor deposition (CVD). Vaporizer structures may be used to provide a means of transferring relatively involatile source reagents or reagent solutions into CVD reactors and often are high surface area, highly efficient heat transfer structures. When vaporizers are used in CVD, often some premature decomposition of the source reagent occurs on the vaporizer element as well as some oxidative decomposition to produce solid products which cause clogging and inefficient vaporization. The invention provides both apparatus and method to periodically flush clean such vaporizer elements to increase their consistency, reliability, and average time between servicings.

    摘要翻译： 一种用于保护源试剂蒸发器结构免受在化学气相沉积（CVD）期间发生的固体积聚的有害影响的方法和方法。 蒸发器结构可用于提供将相对非挥发性的源试剂或试剂溶液转移到CVD反应器中并且通常是高表面积，高效传热结构的方法。 当CVD中使用蒸发器时，通常会在蒸发器元件上发生一些源分解器的过早分解以及一些氧化分解，产生固体产物，导致堵塞和无效蒸发。 本发明提供了周期性地清洗这种蒸发器元件以提高它们的一致性，可靠性和服务之间的平均时间的装置和方法。

    Growth of BaSrTiO.sub.3 using polyamine-based precursors
    4.
    发明授权
    Growth of BaSrTiO.sub.3 using polyamine-based precursors 失效
    使用多胺类前体生长BaSrTiO3

    公开(公告)号：US5919522A

    公开(公告)日：1999-07-06

    申请号：US835768

    申请日：1997-04-08

    申请人： Thomas H. Baum ,  Gregory T. Stauf ,  Peter S. Kirlin ,  Duncan W. Brown ,  Robin A. Gardiner ,  Gautam Bhandari ,  Brian A. Vaartstra

    发明人： Thomas H. Baum ,  Gregory T. Stauf ,  Peter S. Kirlin ,  Duncan W. Brown ,  Robin A. Gardiner ,  Gautam Bhandari ,  Brian A. Vaartstra

    IPC分类号： C07C49/12 ,  C07C211/14 ,  C23C16/18 ,  C23C16/40 ,  C23C16/448 ,  C23C16/00

    CPC分类号： C23C16/18 ,  C23C16/40 ,  C23C16/409 ,  C23C16/4481

    摘要： A method of forming a thin film of BaSrTiO.sub.3 on a substrate in a chemical vapor deposition zone, with transport of a metal precursor composition for the metal-containing film to the chemical vapor deposition zone via a liquid delivery apparatus including a vaporizer. A liquid precursor material is supplied to the liquid delivery apparatus for vaporization thereof to yield the vapor-phase metal precursor composition. The vapor-phase metal precursor composition is flowed to the chemical vapor deposition zone for deposition of metal on the substrate to form the metal-containing film. The liquid precursor material includes a metalorganic polyamine complex, the use of which permits the achievement of sustained operation of the liquid delivery chemical vapor deposition process between maintenance events, due to the low decomposition levels achieved in the vaporization of the polyamine-complexed precursor.

    摘要翻译： 一种在化学气相沉积区中在衬底上形成BaSrTiO3薄膜的方法，该方法通过包括蒸发器的液体输送装置将含金属膜的金属前体组合物输送到化学气相沉积区。 将液体前体材料供给到液体输送装置中以使其蒸发以产生气相金属前体组合物。 气相金属前体组合物流到化学气相沉积区，用于在基底上沉积金属以形成含金属膜。 液体前体材料包括金属有机多胺络合物，其用途允许在维持事件之间实现液体输送化学气相沉积工艺的持续操作，这是由于在多胺络合的前体的蒸发中实现的低分解水平。

    Apparatus for flash vaporization delivery of reagents
    7.
    发明授权
    Apparatus for flash vaporization delivery of reagents 失效
    用于闪蒸的试剂装置

    公开(公告)号：US5536323A

    公开(公告)日：1996-07-16

    申请号：US280143

    申请日：1994-07-25

    申请人： Peter S. Kirlin ,  Robin L. Binder ,  Robin A. Gardiner ,  Peter V. Buskirk ,  Jiming Zhang ,  Gregory Stauf

    发明人： Peter S. Kirlin ,  Robin L. Binder ,  Robin A. Gardiner ,  Peter V. Buskirk ,  Jiming Zhang ,  Gregory Stauf

    IPC分类号： C23C16/18 ,  C23C16/40 ,  C23C16/448 ,  H01L39/24 ,  C23C16/00

    CPC分类号： C23C16/4483 ,  C23C16/18 ,  C23C16/40 ,  C23C16/408 ,  C23C16/409 ,  C23C16/4481 ,  C23C16/45561 ,  H01L39/2441 ,  Y10S261/65 ,  Y10S261/88

    摘要： A process and apparatus for delivering an involatile reagent in gaseous form, wherein an involatile reagent source liquid is flash vaporized on a vaporization matrix structure at elevated temperature. A carrier gas may be flowed past the flash vaporzation matrix structure to yield a carrier gas mixture containing the flash vaporized source reagent. The matrix structure preferably has a high surface-to-volume ratio, and may sutiably comprise a foraminous matrix element such as screen mesh onto which the reagent source liquid is distributed for flash vaporization. The invention is particularly useful for delivery of Group II reagents and compounds and complexes of early transition metals such as zirconium and hafnium, and may be usefully employed with Group II beta-diketonate source layers, e.g., of YBaCuO, BiSrCaCuO, and TlBaCaCuO types, as well as for forming interlayers of Group II metal fluorides between superconductor or gallium arsenide overlayers, and for depositing thin films of photonic and ferroelectric materials, e.g., BaTiO.sub.3, Ba.sub.x Sr.sub.1-x Nb.sub.2 O.sub.6, and PbZr.sub.1-x Ti.sub.x O.sub.3.

    摘要翻译： 一种用于递送气态非挥发性试剂的方法和装置，其中非挥发性试剂源液体在升高的温度下在汽化基质结构上闪蒸。 载气可以流过闪蒸气化基质结构以产生含有闪蒸的源试剂的载气混合物。 基质结构优选具有高的表面体积比，并且可以适当地包含诸如筛网的多孔基质元素，其上分配有试剂源液体用于闪蒸。 本发明特别可用于递送II族试剂和早期过渡金属如锆和铪的化合物和络合物，并且可以有用地用于IIB型β-二酮源层，例如YBaCuO，BiSrCaCuO和TlBaCaCuO类型， 以及用于在超导体或砷化镓覆盖层之间形成第II族金属氟化物的夹层，以及用于沉积光致电子和铁电材料的薄膜，例如BaTiO3，BaxSr1-xNb2O6和PbZr1-xTixO3。

    Metal complex source reagents for MOCVD
    8.
    发明授权
    Metal complex source reagents for MOCVD 失效
    用于MOCVD的金属络合物源试剂

    公开(公告)号：US5453494A

    公开(公告)日：1995-09-26

    申请号：US181800

    申请日：1994-01-18

    申请人： Peter S. Kirlin ,  Duncan W. Brown ,  Robin A. Gardiner

    发明人： Peter S. Kirlin ,  Duncan W. Brown ,  Robin A. Gardiner

    IPC分类号： C23C16/18 ,  C23C16/40 ,  C23C16/448 ,  G01T5/08 ,  G02B6/02 ,  G02B6/036 ,  H01L39/24 ,  C06F5/00 ,  C07D213/22 ,  H01B12/00

    CPC分类号： G02B6/02 ,  C23C16/18 ,  C23C16/40 ,  C23C16/408 ,  C23C16/409 ,  C23C16/4481 ,  C23C16/4483 ,  C23C16/45561 ,  H01L39/2441

    摘要： Metal organic chemical vapor deposition (MOCVD) source reagents useful for formation of metal-containing films, such as thin film copper oxide high temperature superconductor (HTSC) materials. The source reagents have the formula MAyX wherein: M is a metal such as Cu, Ba, Sr, La, Nd, Ce, Pr, Sm, Eu, Th, Gd, Tb, Dy, Ho, Er, Tm Yb, Lu Bi, Tl, Y or Pb; A is a monodentate or multidentate organic ligand; y is 2 or 3; MAy is a stable sub-complex at STP conditions; and X is a monodentate or multidentate ligand coordinated to M and containing one or more atoms independently selected from the group consisting of atoms of the elements C, N, H, S, O, and F. The ligand A may for example be selected from beta-diketonates, cyclopentadienyls, alkyls, perfluoroalkyls, alkoxides, perfluoroalkoxides, and Schiff bases. The complexes of the invention utilize monodentate or multidentate ligands to provide additional coordination to the metal atom, so that the resulting complex is of enhanced volatility characteristics, and enhanced suitability for MOCVD applications.

    摘要翻译： 用于形成含金属膜的金属有机化学气相沉积（MOCVD）源试剂，如薄膜氧化铜高温超导体（HTSC）材料。 所述源试剂具有下式：其中：M是金属如Cu，Ba，Sr，La，Nd，Ce，Pr，Sm，Eu，Th，Gd，Tb，Dy，Ho，Er，Tm Yb，Lu Bi ，Tl，Y或Pb; A是单齿或多齿有机配体; y为2或3; 在STP条件下，MAy是一个稳定的子复合体; 并且X是与M配位且含有独立地选自元素C，N，H，S，O和F的原子的一个或多个原子的单齿或多齿配体。配体A可以例如选自 β-二酮酸酯，环戊二烯基，烷基，全氟烷基，醇盐，全氟烷氧基化物和希夫碱。 本发明的络合物利用单齿或多齿配位体为金属原子提供额外的配位，使得所得复合物具有增强的挥发性特征，并且增强了对MOCVD应用的适用性。

    Method of forming a superconducting oxide layer by MOCVD
    9.
    发明授权
    Method of forming a superconducting oxide layer by MOCVD 失效
    通过MOCVD形成超导氧化物层的方法

    公开(公告)号：US5280012A

    公开(公告)日：1994-01-18

    申请号：US918141

    申请日：1992-07-22

    申请人： Peter S. Kirlin ,  Duncan W. Brown ,  Robin A. Gardiner

    发明人： Peter S. Kirlin ,  Duncan W. Brown ,  Robin A. Gardiner

    IPC分类号： C23C16/18 ,  C23C16/40 ,  C23C16/448 ,  G01T5/08 ,  G02B6/02 ,  G02B6/036 ,  H01L39/24 ,  C23C16/00 ,  B05D5/12

    CPC分类号： C23C16/18 ,  C23C16/40 ,  C23C16/408 ,  C23C16/409 ,  C23C16/4481 ,  C23C16/4483 ,  C23C16/45561 ,  G02B6/02 ,  H01L39/2441 ,  Y10S505/73 ,  Y10S505/734

    摘要： This invention is directed to the metal organic chemical vapor deposition (MOCVD) formation of copper oxide superconductor materials. Various source reagents of Group II elements suitable for high temperature superconductor (HTSC) material formation are described, including beta-diketonates, cyclopentadienyls, alkyls, perfluoroalkyls, alkoxides, perfluoroalkoxides, and Schiff bases, as well as complexes of such Group II compounds, utilizing monodentate or multidentate ligands to provide additional coordination to the Group IIA atom, so that the resulting complex is of enhanced volatility characteristics, and enhanced suitability for MOCVD applications. Also disclosed are methods of synthesizing such compounds and complexes, including a method of making Group II metal beta-diketonate compounds having enhanced thermal stability characteristics.

    摘要翻译： 本发明涉及氧化铜超导材料的金属有机化学气相沉积（MOCVD）的形成。 描述了适用于高温超导体（HTSC）材料形成的II族元素的各种源试剂，包括β-二酮酸酯，环戊二烯基，烷基，全氟烷基，烷氧基，全氟烷氧基和席夫碱，以及这些II族化合物的配合物，利用 单齿或多齿配体，以提供与IIA族原子的额外配位，使得所得复合物具有增强的挥发性特征，并增强了对MOCVD应用的适用性。 还公开了合成这种化合物和络合物的方法，包括制备具有增强的热稳定性特征的II族金属β-二酮化合物的方法。

    Precursor compositions for chemical vapor deposition, and ligand exchange resistant metal-organic precursor solutions comprising same
    10.
    发明授权
    Precursor compositions for chemical vapor deposition, and ligand exchange resistant metal-organic precursor solutions comprising same 失效
    用于化学气相沉积的前体组合物和包含其的配体交换金属 - 有机前体溶液

    公开(公告)号：US5820664A

    公开(公告)日：1998-10-13

    申请号：US414504

    申请日：1995-03-31

    申请人： Robin A. Gardiner ,  Peter S. Kirlin ,  Thomas H. Baum ,  Douglas Gordon ,  Timothy E. Glassman ,  Sofia Pombrik ,  Brian A. Vaartstra

    发明人： Robin A. Gardiner ,  Peter S. Kirlin ,  Thomas H. Baum ,  Douglas Gordon ,  Timothy E. Glassman ,  Sofia Pombrik ,  Brian A. Vaartstra

    IPC分类号： C23C16/18 ,  C23C16/40 ,  C23C16/448 ,  G02B6/036 ,  H01L39/24 ,  C09K3/00

    CPC分类号： H01L39/2441 ,  C23C16/18 ,  C23C16/40 ,  C23C16/408 ,  C23C16/409 ,  C23C16/4481 ,  C23C16/45561 ,  Y10S423/14

    摘要： A metal source reagent liquid solution, comprising: (i) at least one metal coordination complex including a metal to which is coordinatively bound at least one ligand in a stable complex, wherein the ligand is selected from the group consisting of: .beta.-diketonates, .beta.-ketoiminates, .beta.-diiminates, C.sub.1 -C.sub.8 alkyl, C.sub.2 -C.sub.10 alkenyl, C.sub.2 -C.sub.15 cycloalkenyl, C.sub.6 -C.sub.10 aryl, C.sub.1 -C.sub.8 alkoxy, and fluorinated derivatives thereof; and (ii) a solvent for the metal coordination complex. The solutions are usefully employed for chemical vapor deposition of metals from the metal coordination complexes, such as Mg, Ca, Sr, Ba, Sc, Y, La, Ce, Ti, Zr, Hf, Pr, V, Nb, Ta, Nd, Cr, W, Pm, Mn, Re, Sm, Fe, Ru, Eu, Co, Rh, Ir, Gd, Ni, Tb, Cu, Dy, Ho, Al, Tl, Er, Sn, Pb, Tm, Bi, and/or Yb. The solvent may comprise glyme solvents, alkanols, organic ethers, aliphatic hydrocarbons, and/or aromatic hydrocarbons. Solutions of the invention having two or more metal coordination complexes are resistant to detrimental ligand exchange reactions which adversely affect the stability and/or volatilizability of the metal complex for CVD applications.

    摘要翻译： 一种金属源试剂液体溶液，其包含：（i）至少一种金属配位络合物，其包含与稳定络合物中的至少一种配位体配位结合的金属，其中所述配体选自β-二酮化合物， β-酮基，β-二亚胺，C 1 -C 8烷基，C 2 -C 10烯基，C 2 -C 15环烯基，C 6 -C 10芳基，C 1 -C 8烷氧基及其氟化衍生物; 和（ii）金属配位络合物的溶剂。 该溶液有效地用于金属配位络合物如Mg，Ca，Sr，Ba，Sc，Y，La，Ce，Ti，Zr，Hf，Pr，V，Nb，Ta，Nd的金属化学气相沉积 ，Cr，W，Pm，Mn，Re，Sm，Fe，Ru，Eu，Co，Rh，Ir，Gd，Ni，Tb，Cu，Dy，Ho，Al，Tl，Er，Sn，Pb，Tm，Bi ，和/或Yb。 溶剂可以包括甘醇二甲醚溶剂，链烷醇，有机醚，脂族烃和/或芳族烃。 具有两种或更多种金属配位络合物的本发明的溶液对有害的配体交换反应具有抗性，这对于CVD应用的金属络合物的稳定性和/或挥发性是不利的。