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    • 2. 发明授权
    • Preparation of BaFCl:Eu phosphors
    • BaFCl:Eu荧光体的制备
    • US4080306A
    • 1978-03-21
    • US826061
    • 1977-08-19
    • August Ferretti
    • August Ferretti
    • C09K11/77C09K11/46
    • C09K11/7733
    • A process for preparing BaFCl:Eu phosphors of controllable particle size and size distribution is provided. The process comprises (a) preparing an intimate mixture of fine particles of BaFCl, a europium source, preferably water-soluble EuCl.sub.3, and a water-soluble chloride as flux; (b) firing the mixture in an inert atmosphere at a temperature in the range of about 550.degree.-900.degree. C and above the liquid temperature of the flux for a time sufficient to effect reaction and diffusion, and (c) washing the fired product with water to remove the chloride flux. By preselecting the combination of firing temperature and flux concentration in the mixture, phosphor particles of a predetermined size and size distribution can be obtained. This control of the phosphor product is especially advantageous when the intimate mixture is formed in an aqueous medium.
    • 提供了一种制备可控粒径和尺寸分布的BaFCl:Eu荧光粉的方法。 该方法包括(a)制备BaFCl,铕源,优选水溶性EuCl 3的细颗粒和作为助熔剂的水溶性氯化物的紧密混合物; (b)在约550-900℃的温度和高于助熔剂的液体温度的惰性气氛中烧制混合物足够长的时间以进行反应和扩散,和(c)洗涤焙烧产物 用水去除氯化物通量。 通过预先选择混合物中的烧成温度和通量浓度的组合,可以获得预定尺寸和尺寸分布的荧光体颗粒。 当在水性介质中形成紧密混合物时,荧光体产品的这种控制是特别有利的。
    • 3. 发明授权
    • Hydrothermal crystallization vessels
    • 水热结晶容器
    • US5533465A
    • 1996-07-09
    • US376595
    • 1995-01-20
    • August FerrettiOral R. Van Buskirk
    • August FerrettiOral R. Van Buskirk
    • C30B7/00C30B7/10
    • C30B7/00C30B29/10C30B29/14Y10T117/1096
    • A seal apparatus is disclosed for sealing an outlet of a pressurized chamber from fluid loss from the chamber and contamination to the chamber. The apparatus includes certain combinations of (a) a chamber outlet structure; (b) a removable cover; (c) means for reversibly connecting the cover to the chamber outlet structure; and (d) a compressible self-energizing ring having a surface which consists essentially of a material selected from the group consisting of noble metals, noble metal alloys and polytetrafluoroethylene, which has a hardness selected to substantially avoid deformation when the cover is sealed to the chamber outlet structure.Also disclosed are certain pressure vessels for hydrothermal crystal growth using a crystal growth media, which comprise (a) a vessel base and (b) a removable vessel cover. The vessels include (i) certain said combinations employing a compressible self-energizing ring with a surface resistant to corrosion by the crystal growth media and a hardness lower than the hardness of the seal surfaces of the base and cover; and/or (ii) (in an aspect of this invention especially suited for the growth of crystals of the formula MTiOXO.sub.4 wherein M is selected from the group consisting of K, Rb, Tl, NH.sub.4 and mixtures thereof and X is selected from the group consisting of P, As and mixtures thereof) vessel bodies of a nickel alloy essentially free of titanium.
    • 公开了一种密封装置,用于密封加压室的出口,从腔室的流体损失和对室的污染。 该装置包括(a)室出口结构的某些组合; (b)可拆卸盖; (c)用于可逆地将盖连接到室出口结构的装置; 和(d)具有表面的可压缩自增能环,所述表面基本上由选自贵金属,贵金属合金和聚四氟乙烯的材料组成,所述材料具有选择为基本上避免当盖被密封到 室出口结构。 还公开了使用晶体生长介质进行水热晶体生长的某些压力容器,其包括(a)容器基底和(b)可移除的容器盖。 容器包括(i)使用具有耐受结晶生长介质的腐蚀的表面的可压缩自增能环的一些所述组合以及低于基底和盖的密封表面的硬度的硬度; 和/或(ii)(在本发明的一个方面,特别适合于生长式MTiOXO4的晶体,其中M选自K,Rb,Tl,NH 4及其混合物,X选自 由P,As及其混合物组成)基本上不含钛的镍合金的容器体。
    • 5. 发明授权
    • Processes for preparation of ion exchanged crystalline waveguides
    • 制备离子交换晶体波导的方法
    • US5266092A
    • 1993-11-30
    • US894669
    • 1992-06-05
    • John D. BierleinAugust FerrettiMark G. Roelofs
    • John D. BierleinAugust FerrettiMark G. Roelofs
    • G02B6/134C03B37/075B01J17/24
    • G02B6/1345
    • There is disclosed an optical waveguide comprising a K.sub.1-x Rb.sub.x TiOmO.sub.4 single crystal substrate, wherein x is from 0 to 1 and M is P or As, having at least one optically smooth surface wherein sufficient K.sup.+ and/or Rb.sup.+ have been replaced by ions selected from at least one of H.sup.+ and NH.sub.4.sup.+ and, optionally, at least one monovalent ion selected from Rb.sup.+, Cs.sup.+, Tl.sup.+, and/or at least one divalent ion selected from Ba.sup.+2, Sr.sup.+2, Ca.sup.+2 and Pb.sup.+2 to chance the surface index of refraction at least a 0.00025 with respect to the index of refraction of the single crystal substrate. One process disclosed for producing an optical waveguide comprises the steps of contacting at least one optically smooth surface of a single crystal of K.sub.1-x Rb.sub.x TiOmO.sub.4 with an ion exchange medium capable of supplying said replacement ions, at a temperature of from about 100.degree. C. to about 600.degree. C. for a time sufficient to increase the surface index of refraction at least about 0.00025 with respect to the index of refraction of the single crystal by replacing K.sup.+ and/or Rb.sup.+ of said single crystal with said ions supplied by the exchange medium, and cooling the resulting crystal. Another process disclosed for producing an optical waveguide comprises the step of applying a DC voltage of from about 20 V per cm of crystal thickness to about 2000 V per cm of crystal thickness across the z-surfaces of a z-cut K.sub.1-x Rb.sub.x TiOmO.sub.4 single crystal, in the presence of a proton source at a temperature of from about -40.degree. C. to 400.degree. C. for a time sufficient to raise the index of refraction underneath the anode by at least 0.00025 with respect to the index of refraction of the single crystal by replacing K.sup.+ and/or Rb.sup.+ of said single crystal with H.sup.+. A nonlinear optic device using the optical waveguide of the invention is also disclosed.
    • 公开了一种包括K1-xRbxTiOmO4单晶衬底的光波导,其中x为0至1,M为P或As,具有至少一个光学平滑表面,其中足够的K +和/或Rb +已被 选自Rb +,Cs +,Tl +和/或至少一种选自Ba + 2,Sr + 2,Ca + 2和Pb + 2的二价离子中的至少一种H +和NH 4 +,以及任选的至少一种一价离子, 相对于单晶衬底的折射率,表面折射率几率为0.00025以上。 公开的用于制造光波导的一个方法包括以下步骤:将K1-xRbxTiOmO4的单晶的至少一个光学光滑表面与能够提供所述置换离子的离子交换介质在约100℃至 约600℃,足以通过用由交换介质提供的所述离子代替所述单晶的K +和/或Rb +而使表面折射率相对于单晶的折射率提高至少约0.00025的时间 ,并冷却所得晶体。 公开的用于制造光波导的另一方法包括以下步骤:在z切割的K1-xRbxTiOmO4单晶的z面上施加约20V / cm晶体厚度的直流电压至约2000V / cm的晶体厚度 在质子源的存在下,在约-40℃至400℃的温度下,足以使阳极下方的折射率相对于折射率的至少0.00025提高的时间 通过用H +代替所述单晶的K +和/或Rb +的单晶。 还公开了使用本发明的光波导的非线性光学装置。
    • 8. 发明授权
    • Process for spheroidal BaFCl:Eu phosphor particles
    • 球形BaFCl:Eu荧光体颗粒的工艺
    • US4524016A
    • 1985-06-18
    • US509324
    • 1983-06-28
    • August Ferretti
    • August Ferretti
    • C09K11/77C09K11/465
    • C09K11/7733
    • Process for preparing spheroidal particulate BaFCl:Eu phosphor having a narrow size distribution, which process comprises:(a) spray drying the slurry comprised of BaFCl, or the precursors thereof, a europium halide, and a BaCl.sub.2 flux in a liquid under conditions which produce porous spheroidal agglomerates of BaFCl, or the precursors thereof, BaCl.sub.2, and the europium halide, the agglomerates having an average diameter larger than the desired diameter of the particulate phosphor;(b) firing the porous spheroidal agglomerates of step (a) in a flowing inert atmosphere for about 10 to about 120 minutes at a temperature of about 650.degree. C. to about 950.degree. C.;(c) cooling the fired material of step (b) to ambient temperature in an inert atmosphere;(d) washing the cooled material of step (c) with water to remove BaCl.sub.2 ; and(e) drying the washed material of step (d) to remove the water and to produce the free flowing powder comprised of spheroidal particulate BaFCl:Eu phosphor.
    • 制备具有窄尺寸分布的球形颗粒BaFCl:Eu荧光体的方法,该方法包括:(a)在产生BaFCl或其前体的浆料,卤化铕和BaCl 2助熔剂的液体中,在产生 BaFCl或其前体BaCl 2和卤化铕的多孔球形聚集体具有平均直径大于颗粒状荧光体的期望直径的平均直径; (b)在约650℃至约950℃的温度下,在流动的惰性气氛中焙烧步骤(a)的多孔球状凝聚体约10至约120分钟; (c)在惰性气氛中将步骤(b)的烧制材料冷却至环境温度; (d)用水洗涤步骤(c)的冷却材料以除去BaCl 2; 和(e)干燥步骤(d)的洗涤材料以除去水并产生由球形颗粒BaFCl:Eu荧光体组成的自由流动的粉末。
    • 10. 发明授权
    • Process for the production of Ba(Sr)FCl:Eu phosphors
    • 制备Ba(Sr)FCl:Eu荧光体的方法
    • US3988252A
    • 1976-10-26
    • US522880
    • 1974-11-11
    • August Ferretti
    • August Ferretti
    • C09K11/77C09K11/46
    • C09K11/7791
    • Phosphors of the formula Ba.sub.1-x-y-z Sr.sub.x Eu.sub.y R.sub.z FCl when R is one or more of Sm, Dy, Sb, Bi or Zn, x is from 0 to 0.1, y is from 0.0001 to 0.2 and z is from 0 to 0.1 having high efficiency and low lag are made by (1) intimately mixing a substantially stoichiometric mixture of the appropriate metal halides having at least 30% of particles less than 1.5.mu. with the remaining particles having an average particle size less than 3.mu. (2) firing in an atmosphere free of hydrogen at 600.degree. to 950.degree. C for a time sufficient to effect reaction and (3) pulverizing the sintered product. Suitable intimate mixtures of the starting materials can be prepared by (a) prolonged ball milling of the ingredients in the presence of certain organic liquids followed by filtration and drying or (b) slurrying insoluble fluoride powders with an aqueous solution of soluble chloride powders followed by precipitation with an excess of a water miscible organic solvent or (c) freeze-drying a thick aqueous slurry of the ingredients.
    • 当R为Sm,Dy,Sb,Bi或Zn中的一种或多种时,式Ba1-xy-zSrxEuyRzFCl的荧光体为x为0〜0.1,y为0.0001〜0.2,z为0〜0.1, 通过(1)将具有至少30%的小于1.5μm的颗粒的适当金属卤化物的基本上化学计量的混合物与平均粒径小于3μm的剩余颗粒(2)充分混合,制成低滞后气氛 在600-950℃下不含氢气足以进行反应的时间和(3)粉碎烧结产品。 起始材料的合适的紧密混合物可以通过以下步骤制备:(a)在某些有机液体存在下对组分进行长时间的研磨,然后过滤和干燥,或(b)用不溶性氟化物粉末与可溶性氯化物粉末水溶液 用过量的水混溶性有机溶剂沉淀,或(c)冷冻干燥成分浓稠的含水浆液。