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    • 5. 发明授权
    • Dehydration and purification of isopropyl alcohol to an ultradry and
ultrapure level
    • 脱水和纯化异丙醇超纯超纯水平
    • US5868906A
    • 1999-02-09
    • US691427
    • 1996-08-02
    • John A. AdamsGerald A. KrulikChristopher BlattDavid Persichini
    • John A. AdamsGerald A. KrulikChristopher BlattDavid Persichini
    • B01D3/14B01D61/36C07C29/80C07C29/82C07C31/10B01D3/00
    • B01D61/362B01D3/146C07C29/80C07C29/82Y10S159/27Y10S203/17
    • A method for the on-site reprocessing of isopropyl alcohol used in semiconductor manufacturing, to generate an ultradry and ultrapure isopropyl alcohol. This ultradry and ultrapure isopropyl alcohol is produced through a pervaporation step, followed by double distillation. In the first distillation step, an autonomous azeotropic self-stripping distillation column is used to produce an ultradry and partially purified isopropyl alcohol. In the next step, the isopropyl alcohol is distilled in an overhead product distillation column, to produce an ultrapure and ultradry isopropyl alcohol. Alternatively, if the feed isopropyl alcohol contains less than 2000 ppm water, the pervaporation step may be omitted.The resulting isopropyl alcohol has between a high of 100 parts per million (ppm) and a low of 0.1 ppm of water in the isopropyl alcohol. It also has zero particles per milliliter of a size larger than 2.0 microns, zero to 2 particles per milliliter of a size of 0.5 micron to 2.0 microns, zero to 30 particles per milliliter of a size between 0.1 microns and 0.5 microns, an unspecified number of particles per milliliter below 0.1 microns, 1 part per trillion (ppt) to 1 part per billion (ppb) of any specific trace impurity such as metals, anions, and cations, and 10 ppt to 10 ppm of any other specific trace organic substances.
    • 用于半导体制造中的异丙醇的现场再处理方法,以产生超纯和超纯异丙醇。 通过全蒸发步骤生产超纯超纯异丙醇,然后进行双蒸馏。 在第一蒸馏步骤中,使用自主共沸自剥离蒸馏塔来生产超纯和部分纯化的异丙醇。 在下一步骤中,将异丙醇在塔顶馏出物蒸馏塔中蒸馏,生成超纯和超纯异丙醇。 或者,如果进料异丙醇含有少于2000ppm的水,则可以省略渗透蒸发步骤。 得到的异丙醇在异丙醇中的百万分之100ppm(ppm)和0.1ppm的低含量之间。 它还具有每毫升小于2.0微米的零颗粒,每毫升为零至2微米的0.5微米至2.0微米的零微粒,每毫升0.1微米至0.5微米之间的每毫升为零至30微米,未指定数量 每毫升0.1微米以下的颗粒,每万亿分之1份(ppt)至十亿分之一(ppb)的任何特定痕量杂质如金属,阴离子和阳离子,10磅至10ppm的任何其他特定微量有机物质 。
    • 7. 发明授权
    • Separation and purification of fluoride from industrial wastes
    • 从工业废物中分离和纯化氟化物
    • US5876685A
    • 1999-03-02
    • US707907
    • 1996-09-11
    • Gerald A. KrulikJohn A. AdamsDieter DornischDavid W. PersichiniChristopher S. Blatt
    • Gerald A. KrulikJohn A. AdamsDieter DornischDavid W. PersichiniChristopher S. Blatt
    • B01D15/04C01B7/19C02F1/04C02F1/42C02F1/58C02F1/60C02F1/66C02F9/00
    • C02F9/00C01B7/191C01B7/196C02F1/583C02F1/60C02F1/04C02F1/42C02F1/66C02F2101/14C02F2103/346
    • A method for the removal and purification of substantially all of the fluoride ions contained in a solution containing greater than 10 parts per million (ppm) fluoride ion, a mixture of other anions, silicon in the form of a fluorosilicic acid, silicic acid, silicates, or silicon tetrafluoride, and optionally also containing complex metal fluorides, to produce an ultrapure hydrofluoric acid, comprising the steps of (a) adjusting the pH of the solution to an alkaline pH to hydrolyze the fluorosilicic acid and any complex metal fluorides; (b) removing the fluoride ions and other anions from the solution by passing the solution through an ion exchange resin, where the ion exchange resin is adapted to adsorb substantially all of the fluoride passed over the ion exchange resin; (c) displacing the fluoride ions and other anions bound to the ion exchange resin, thereby forming a mixture of anions in an effluent emanating from resin; (d) optionally concentrating the effluent at a high pH and then lowering the pH; and (e) distilling the mixture of anions in the effluent from a sulfuric acid solution to generate ultrapure hydrofluoric acid. An apparatus useful for practicing the method is also disclosed.
    • 除去和纯化含有大于10ppm(ppm)氟离子,其它阴离子的混合物,氟硅酸形式的硅,硅酸,硅酸盐的溶液中所含的基本上所有的氟离子的方法 ,或四氟化硅,以及任选地还含有复合金属氟化物,以制备超纯氢氟酸,包括以下步骤:(a)将溶液的pH调节至碱性pH以水解氟硅酸和任何复合金属氟化物; (b)通过使溶液通过离子交换树脂从溶液中除去氟离子和其它阴离子,其中离子交换树脂适于吸附通过离子交换树脂的基本上所有的氟化物; (c)置换与离子交换树脂结合的氟离子和其它阴离子,从而在由树脂发出的流出物中形成阴离子的混合物; (d)任选地在高pH下浓缩流出物,然后降低pH值; 和(e)将来自硫酸溶液的流出物中的阴离子混合物蒸馏以产生超纯氢氟酸。 还公开了一种用于实施该方法的装置。
    • 9. 发明授权
    • Recycle process for regeneration of ammoniacal copper etchant
    • 氨铜腐蚀剂再生回收工艺
    • US5556553A
    • 1996-09-17
    • US447752
    • 1995-05-23
    • Gerald A. KrulikNenad V. MandichRajwant Singh
    • Gerald A. KrulikNenad V. MandichRajwant Singh
    • C23F1/46B44C1/22C23F1/00
    • C23F1/46
    • A process for control of recycle of ammoniacal copper etchant which uses metallic aluminum to remove copper without substantially adding undesirable byproducts, by controlling the temperature and mixture rate of the removal process. The very rapid reaction can be controlled by using a diluent of copper-free etchant, heating to process temperature, then adding spent, copper containing etchant at a controlled rate while actively cooling the system to control the temperature. The copper concentration can be monitored by colorimetry while maintaining the pH above pH 8. The separated metallic copper and aluminum hydroxide sludge are easily filtered from the etchant. The purified etchant is now suitable for chemical adjustment and reuse.
    • 用于控制氨铜腐蚀剂的再循环的方法,其通过控制除去过程的温度和混合速率,其使用金属铝去除铜而基本上不加入不需要的副产物。 可以通过使用无铜蚀刻剂的稀释剂,加热至加工温度,然后以有控制的速率加入废铜的蚀刻剂,同时主动冷却系统以控制温度,来控制非常快的反应。 可以通过比色法监测铜浓度,同时保持pH高于pH8。分离的金属铜和氢氧化铝污泥容易从蚀刻剂中过滤。 纯化的蚀刻剂现在适用于化学调整和再利用。
    • 10. 发明授权
    • Solder and tin stripper composition
    • 锡和锡剥离剂组合物
    • US5512201A
    • 1996-04-30
    • US388444
    • 1995-02-13
    • Rajwant SinghNenad MandichGerald A. Krulik
    • Rajwant SinghNenad MandichGerald A. Krulik
    • C23F1/44C23D1/00
    • C23F1/44
    • A metal dissolving liquid and method for stripping tin and solder coatings, including the underlying tin-copper alloy, from the copper substrate of a printed circuit board. The liquid includes an aqueous solution of nitric acid in an amount sufficient to dissolve solder and tin, a source of ferric ions in an amount sufficient to dissolve tin-copper alloy, a source of halide ions in an amount sufficient to solubilize tin, an effective amount of methylsulfonic acid as promoter for complete stripping, and a source of an organic, water soluble amine. The combination of ingredients will substantially eliminate sludge formation, reduce attack on the copper substrate and provide a bright copper finish after solder removal. A liquid further including organic triazoles including benzotriazole in amounts not more than about 5% by weight and sulfamic ions in amounts not more than about 2.5% by weight.
    • 一种金属溶解液以及从印刷电路板的铜基底上剥离锡和焊料涂层(包括下面的锡 - 铜合金)的方法。 该液体包括硝酸水溶液,其量足以溶解锡和锡,铁离子源的量足以溶解锡 - 铜合金,卤素源的量足以溶解锡,有效 甲基磺酸的量作为完全汽提的促进剂,以及有机水溶性胺的来源。 成分的组合将基本上消除污泥形成,减少对铜基材的侵蚀并且在去除焊料后提供亮的铜表面。 进一步包括含量不超过约5重量%的有机三唑(包括苯并三唑)和不超过约2.5重量%的氨基磺酸根离子的液体。