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公开(公告)号：US09371226B2
公开(公告)日：2016-06-21
申请号：US13019879
申请日：2011-02-02
申请人： Robert V. Fox , Fengyan Zhang , Rene G. Rodriguez , Joshua J. Pak , Chivin Sun
发明人： Robert V. Fox , Fengyan Zhang , Rene G. Rodriguez , Joshua J. Pak , Chivin Sun
IPC分类号： H01L31/02 , H01L31/18 , C01B17/00 , B82Y30/00 , C01G15/00 , H01L31/032 , H01L31/0392 , H01L31/0749
CPC分类号： B82Y30/00 , C01G15/006 , C01P2002/72 , C01P2002/84 , C01P2004/62 , C01P2004/64 , C01P2006/40 , H01L31/0322 , H01L31/03923 , H01L31/0749 , Y02E10/541
摘要： Single source precursors or pre-copolymers of single source precursors are subjected to microwave radiation to form particles of a I-III-VI2 material. Such particles may be formed in a wurtzite phase and may be converted to a chalcopyrite phase by, for example, exposure to heat. The particles in the wurtzite phase may have a substantially hexagonal shape that enables stacking into ordered layers. The particles in the wurtzite phase may be mixed with particles in the chalcopyrite phase (i.e., chalcopyrite nanoparticles) that may fill voids within the ordered layers of the particles in the wurtzite phase thus produce films with good coverage. In some embodiments, the methods are used to form layers of semiconductor materials comprising a I-III-VI2 material. Devices such as, for example, thin-film solar cells may be fabricated using such methods.
摘要翻译： 将单源前体或单源前体的预共聚物进行微波辐射以形成I-III-VI2材料的颗粒。 这样的颗粒可以以纤锌矿相形成，并且可以通过例如暴露于热而转变成黄铜矿相。 纤锌矿相中的颗粒可以具有基本上六边形的形状，其能够堆叠成有序层。 纤锌矿相中的颗粒可以与黄铜矿相中的颗粒（即，黄铜矿纳米颗粒）混合，其可以填充纤锌矿相中颗粒的有序层内的空隙，从而产生具有良好覆盖率的膜。 在一些实施例中，所述方法用于形成包含I-III-VI2材料的半导体材料层。 可以使用这样的方法来制造诸如薄膜太阳能电池的装置。
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公开(公告)号：US08951446B2
公开(公告)日：2015-02-10
申请号：US13365800
申请日：2012-02-03
申请人： Robert V. Fox , Rene Rodriguez , Joshua J. Pak , Chivin Sun
发明人： Robert V. Fox , Rene Rodriguez , Joshua J. Pak , Chivin Sun
IPC分类号： H01B1/02
CPC分类号： C01B17/20 , B82Y30/00 , C01B19/002 , C01P2002/30 , C01P2004/62 , C01P2004/64 , C01P2004/80 , C01P2006/80
摘要： Hybrid particles that comprise a coating surrounding a chalcopyrite material, the coating comprising a metal, a semiconductive material, or a polymer; a core comprising a chalcopyrite material and a shell comprising a functionalized chalcopyrite material, the shell enveloping the core; or a reaction product of a chalcopyrite material and at least one of a reagent, heat, and radiation. Methods of forming the hybrid particles are also disclosed.
摘要翻译： 包含围绕黄铜矿材料的涂层的混合颗粒，所述涂层包含金属，半导体材料或聚合物; 包含黄铜矿材料的核心和包含官能化黄铜矿材料的壳体，所述壳体包围所述核心; 或黄铜矿材料与试剂，热和辐射中的至少一种的反应产物。 还公开了形成杂化颗粒的方法。
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公开(公告)号：US20130060054A1
公开(公告)日：2013-03-07
申请号：US13659620
申请日：2012-10-24
申请人： Robert V.Fox , Rene G. Rodriguez , Joshua J. Pak , Chivin Sun , Kelsey R. Margulieux , Andrew W. Holland , BATTELLE ENERGY ALLIANCE, LLC
发明人： Robert V. Fox , Rene G. Rodriguez , Joshua J. Pak , Chivin Sun , Kelsey R. Margulieux , Andrew W. Holland
IPC分类号： C07F19/00
CPC分类号： C07F9/5045 , C07F19/005
摘要： Methods of forming single source precursors (SSPs) include forming intermediate products having the empirical formula ½{L2N(μ-X)2M′X2}2, and reacting MER with the intermediate products to form SSPs of the formula L2N(μ-ER)2M′(ER)2, wherein L is a Lewis base, M is a Group IA atom, N is a Group IB atom, M′ is a Group IIIB atom, each E is a Group VIB atom, each X is a Group VIIA atom or a nitrate group, and each R group is an alkyl, aryl, vinyl, (per)fluoro alkyl, (per)fluoro aryl, silane, or carbamato group. Methods of forming polymeric or copolymeric SSPs include reacting at least one of HE1R1E1H and MER with one or more substances having the empirical formula L2N(μ-ER)2M′(ER)2 or L2N(μ-X)2M′(X)2 to form a polymeric or copolymeric SSP. New SSPs and intermediate products are formed by such methods.
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4.发明申请FORMATION OF INTEGRAL COMPOSITE PHOTON ABSORBER LAYER USEFUL FOR PHOTOACTIVE DEVICES AND SENSORS 审中-公开形成用于光电器件和传感器的整体复合光子吸收层公开(公告)号：US20130026535A1
公开(公告)日：2013-01-31
申请号：US13191062
申请日：2011-07-26
申请人： Robert V. Fox , Rene G. Rodriguez , Joshua J. Pak
发明人： Robert V. Fox , Rene G. Rodriguez , Joshua J. Pak
CPC分类号： H01L31/0322 , B82Y20/00 , B82Y30/00 , G02B2207/101 , H01L31/0384 , H01L31/03923 , H01L31/0749 , Y02E10/541
摘要： Methods of forming photoactive devices include infiltrating pores of a solid porous ceramic material with a fluid, which may be a supercritical fluid, carrying at least one single source precursor therein. The single source precursor may be decomposed to form a plurality of particles within the pores of the solid porous ceramic material. Photoactive devices include a solid porous ceramic material exhibiting electrical conductivity, and a plurality of photoactive semiconductor particles within pores of the solid porous ceramic material.
摘要翻译： 形成光活性器件的方法包括具有流体的固体多孔陶瓷材料的渗透孔，流体可以是超临界流体，其中至少携带一个单一的源前体。 单源前体可以分解成在固体多孔陶瓷材料的孔内形成多个颗粒。 光活性器件包括表现出导电性的固体多孔陶瓷材料和固体多孔陶瓷材料孔内的多个光活性半导体颗粒。
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5.发明授权Methods of forming single source precursors, methods of forming polymeric single source precursors, and single source precursors and intermediate products formed by such methods 有权形成单源前体的方法，形成聚合单源前体的方法，以及通过这些方法形成的单源前体和中间产物公开(公告)号：US08324414B2
公开(公告)日：2012-12-04
申请号：US12646474
申请日：2009-12-23
申请人： Robert V. Fox , Rene G. Rodriguez , Joshua J. Pak , Chivin Sun , Kelsey R. Margulieux , Andrew W. Holland
发明人： Robert V. Fox , Rene G. Rodriguez , Joshua J. Pak , Chivin Sun , Kelsey R. Margulieux , Andrew W. Holland
CPC分类号： C07F9/5045 , C07F19/005
摘要： Methods of forming single source precursors (SSPs) include forming intermediate products having the empirical formula ½{L2N(μ-X)2M′X2}2, and reacting MER with the intermediate products to form SSPs of the formula L2N(μ-ER)2M′(ER)2, wherein L is a Lewis base, M is a Group IA atom, N is a Group IB atom, M′ is a Group IIIB atom, each E is a Group VIB atom, each X is a Group VIIA atom or a nitrate group, and each R group is an alkyl, aryl, vinyl, (per)fluoro alkyl, (per)fluoro aryl, silane, or carbamato group. Methods of forming polymeric or copolymeric SSPs include reacting at least one of HE1R1E1H and MER with one or more substances having the empirical formula L2N(μ-ER)2M′(ER)2 or L2N(μ-X)2M′(X)2 to form a polymeric or copolymeric SSP. New SSPs and intermediate products are formed by such methods.
摘要翻译： 形成单源前体（SSPs）的方法包括形成具有经验式½{L2N（μ-X）2M'X2} 2的中间产物，并使MER与中间产物反应形成式L2N（μ-ER）的SSP， 2M'（ER）2，其中L是路易斯碱，M是IA族原子，N是IB族原子，M'是IIIB原子，每个E是VIB族原子，每个X是VIIA族 原子或硝酸根，每个R基团是烷基，芳基，乙烯基，（全）氟烷基，（全）氟芳基，硅烷或氨基甲酰基。 形成聚合物或共聚物SSP的方法包括使HE1R1E1H和MER中的至少一种与一种或多种具有经验式L2N（μ-ER）2M'（ER）2或L2N（μ-X）2M'（X）2 以形成聚合物或共聚物SSP。 通过这种方法形成新的SSP和中间产品。
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6.发明申请METHODS OF FORMING SINGLE SOURCE PRECURSORS, METHODS OF FORMING POLYMERIC SINGLE SOURCE PRECURSORS, AND SINGLE SOURCE PRECURSORS AND INTERMEDIATE PRODUCTS FORMED BY SUCH METHODS 有权形成单一来源前体的方法，形成聚合单体源前体的方法，单源资源前体和通过这些方法形成的中间产物公开(公告)号：US20110152554A1
公开(公告)日：2011-06-23
申请号：US12646474
申请日：2009-12-23
申请人： Robert V. Fox , Rene G. Rodriguez , Joshua J. Pak , Chivin Sun , Kelsey R. Margulieux , Andrew W. Holland
发明人： Robert V. Fox , Rene G. Rodriguez , Joshua J. Pak , Chivin Sun , Kelsey R. Margulieux , Andrew W. Holland
IPC分类号： C07F1/08
CPC分类号： C07F9/5045 , C07F19/005
摘要： Methods of forming single source precursors (SSPs) include forming intermediate products having the empirical formula ½{L2N(μ-X)2M′X2}2, and reacting MER with the intermediate products to form SSPs of the formula L2N(μ-ER)2M′(ER)2, wherein L is a Lewis base, M is a Group IA atom, N is a Group IB atom, M′ is a Group IIIB atom, each E is a Group VIB atom, each X is a Group VIIA atom or a nitrate group, and each R group is an alkyl, aryl, vinyl, (per)fluoro alkyl, (per)fluoro aryl, silane, or carbamato group. Methods of forming polymeric or copolymeric SSPs include reacting at least one of HE1R1E1H and MER with one or more substances having the empirical formula L2N(μ-ER)2M′(ER)2 or L2N(μ-X)2M′(X)2 to form a polymeric or copolymeric SSP. New SSPs and intermediate products are formed by such methods.
摘要翻译： 形成单源前体（SSPs）的方法包括形成具有经验式½{L2N（μ-X）2M'X2} 2的中间产物，并使MER与中间产物反应形成式L2N（μ-ER）的SSP， 2M'（ER）2，其中L是路易斯碱，M是IA族原子，N是IB族原子，M'是IIIB原子，每个E是VIB族原子，每个X是VIIA族 原子或硝酸根，每个R基团是烷基，芳基，乙烯基，（全）氟烷基，（全）氟芳基，硅烷或氨基甲酰基。 形成聚合物或共聚物SSP的方法包括使HE1R1E1H和MER中的至少一种与一种或多种具有经验式L2N（μ-ER）2M'（ER）2或L2N（μ-X）2M'（X）2 以形成聚合物或共聚物SSP。 通过这种方法形成新的SSP和中间产品。
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7.发明申请RAPID SYNTHESIS AND SIZE CONTROL OF CHALCOPYRITE-BASED SEMI-CONDUCTOR NANOPARTICLES USING MICROWAVE IRRADIATION 有权使用微波辐射法快速合成和基于聚合物的半导体纳米粒子的尺寸控制公开(公告)号：US20110017017A1
公开(公告)日：2011-01-27
申请号：US11957108
申请日：2007-12-14
CPC分类号： C30B7/14 , C22B4/06 , C30B29/46 , C30B29/605 , C30B30/00 , H01L31/0322 , Y02E10/541 , Y02P70/521 , Y10S977/813
摘要： CuInS2 nanoparticles have been prepared from single source precursors via microwave irradiation. Also, CuInGaS2 alloy nanoparticles have been prepared. Microwave irradiation methods have allowed an increase in the efficiency of preparation of these materials by providing increased uniformity of heating and shorter reaction times. Nanoparticle growth has been controlled in the about 1 to 5 nm size range by variation of thiolated capping ligand concentrations as well as reaction temperatures and times. Investigation of the photophysical properties of the colloidal nanoparticles has been performed using electronic absorption and luminescence emission spectroscopy. Qualitative nanoparticles sizes have been determined from the photoluminescence (PL) data and compared to TEM images.
摘要翻译： 已经通过微波照射从单源前体制备了CuInS 2纳米颗粒。 此外，还制备了CuInGaS2合金纳米颗粒。 通过提供增加的加热均匀性和较短的反应时间，微波照射方法允许提高这些材料的制备效率。 通过硫醇化封端配体浓度以及反应温度和时间的变化，纳米颗粒生长被控制在约1至5nm尺寸范围内。 使用电子吸收和发光发射光谱法进行胶体纳米粒子的光物理性质的研究。 已经从光致发光（PL）数据确定了定性纳米颗粒尺寸，并与TEM图像进行了比较。
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公开(公告)号：US20130200313A1
公开(公告)日：2013-08-08
申请号：US13365800
申请日：2012-02-03
申请人： ROBERT V. FOX , RENE RODRIGUEZ , JOSHUA J. PAK , CHIVIN SUN
发明人： ROBERT V. FOX , RENE RODRIGUEZ , JOSHUA J. PAK , CHIVIN SUN
CPC分类号： C01B17/20 , B82Y30/00 , C01B19/002 , C01P2002/30 , C01P2004/62 , C01P2004/64 , C01P2004/80 , C01P2006/80
摘要： Hybrid particles that comprise a coating surrounding a chalcopyrite material, the coating comprising a metal, a semiconductive material, or a polymer; a core comprising a chalcopyrite material and a shell comprising a functionalized chalcopyrite material, the shell enveloping the core; or a reaction product of a chalcopyrite material and at least one of a reagent, heat, and radiation. Methods of forming the hybrid particles are also disclosed.
摘要翻译： 包含围绕黄铜矿材料的涂层的混合颗粒，所述涂层包含金属，半导体材料或聚合物; 包含黄铜矿材料的核心和包含官能化黄铜矿材料的壳体，所述壳体包围所述核心; 或黄铜矿材料与试剂，热和辐射中的至少一种的反应产物。 还公开了形成杂化颗粒的方法。
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9.发明授权Rapid synthesis and size control of chalcopyrite-based semi-conductor nanoparticles using microwave irradiation 有权使用微波照射快速合成和控制黄铜矿基半导体纳米粒子公开(公告)号：US07892519B2
公开(公告)日：2011-02-22
申请号：US11957108
申请日：2007-12-14
IPC分类号： C01B17/00
CPC分类号： C30B7/14 , C22B4/06 , C30B29/46 , C30B29/605 , C30B30/00 , H01L31/0322 , Y02E10/541 , Y02P70/521 , Y10S977/813
摘要： CuInS2 nanoparticles have been prepared from single source precursors via microwave irradiation. Also, CuInGaS2 alloy nanoparticles have been prepared. Microwave irradiation methods have allowed an increase in the efficiency of preparation of these materials by providing increased uniformity of heating and shorter reaction times. Nanoparticle growth has been controlled in the about 1 to 5 nm size range by variation of thiolated capping ligand concentrations as well as reaction temperatures and times. Investigation of the photophysical properties of the colloidal nanoparticles has been performed using electronic absorption and luminescence emission spectroscopy. Qualitative nanoparticles sizes have been determined from the photoluminescence (PL) data and compared to TEM images.
摘要翻译： 已经通过微波照射从单源前体制备了CuInS 2纳米颗粒。 此外，还制备了CuInGaS2合金纳米颗粒。 通过提供增加的加热均匀性和较短的反应时间，微波照射方法允许提高这些材料的制备效率。 通过硫醇化封端配体浓度以及反应温度和时间的变化，纳米颗粒生长被控制在约1至5nm尺寸范围内。 使用电子吸收和发光发射光谱法进行胶体纳米粒子的光物理性质的研究。 已经从光致发光（PL）数据确定了定性纳米颗粒尺寸，并与TEM图像进行了比较。
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10.发明申请METHODS FOR FORMING PARTICLES, METHODS OF FORMING SEMICONDUCTOR MATERIALS, METHODS OF FORMING SEMICONDUCTOR DEVICES, AND DEVICES FORMED USING SUCH METHODS 有权形成颗粒的方法，形成半导体材料的方法，形成半导体器件的方法和使用这种方法形成的器件公开(公告)号：US20120192930A1
公开(公告)日：2012-08-02
申请号：US13019879
申请日：2011-02-02
申请人： ROBERT V. FOX , FENGYAN ZHANG , RENE G. RODRIGUEZ , JOSHUA J. PAK , CHIVIN SUN
发明人： ROBERT V. FOX , FENGYAN ZHANG , RENE G. RODRIGUEZ , JOSHUA J. PAK , CHIVIN SUN
CPC分类号： B82Y30/00 , C01G15/006 , C01P2002/72 , C01P2002/84 , C01P2004/62 , C01P2004/64 , C01P2006/40 , H01L31/0322 , H01L31/03923 , H01L31/0749 , Y02E10/541
摘要： Single source precursors or pre-copolymers of single source precursors are subjected to microwave radiation to form particles of a I-III-VI2 material. Such particles may be formed in a wurtzite phase and may be converted to a chalcopyrite phase by, for example, exposure to heat. The particles in the wurtzite phase may have a substantially hexagonal shape that enables stacking into ordered layers. The particles in the wurtzite phase may be mixed with particles in the chalcopyrite phase (i.e., chalcopyrite nanoparticles) that may fill voids within the ordered layers of the particles in the wurtzite phase thus produce films with good coverage. In some embodiments, the methods are used to form layers of semiconductor materials comprising a I-III-VI2 material. Devices such as, for example, thin-film solar cells may be fabricated using such methods.
摘要翻译： 将单源前体或单源前体的预共聚物进行微波辐射以形成I-III-VI2材料的颗粒。 这样的颗粒可以以纤锌矿相形成，并且可以通过例如暴露于热而转变成黄铜矿相。 纤锌矿相中的颗粒可以具有基本上六边形的形状，其能够堆叠成有序层。 纤锌矿相中的颗粒可以与黄铜矿相中的颗粒（即，黄铜矿纳米颗粒）混合，其可以填充纤锌矿相中颗粒的有序层内的空隙，从而产生具有良好覆盖率的膜。 在一些实施例中，所述方法用于形成包含I-III-VI2材料的半导体材料层。 可以使用这样的方法来制造诸如薄膜太阳能电池的装置。
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