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1. 发明申请

US20050263399A1 Efficient analysis of organic additives in an acid copper plating bath 失效
标题翻译：酸性镀铜浴中有机添加剂的有效分析
公开(公告)号：US20050263399A1
公开(公告)日：2005-12-01
申请号：US10856619
申请日：2004-05-27
申请人： Eugene Shalyt , Michael Pavlov , Peter Bratin , Alex Kogan , Michael Perpich
发明人： Eugene Shalyt , Michael Pavlov , Peter Bratin , Alex Kogan , Michael Perpich
IPC分类号： C25D3/38 , C25D5/00 , C25D21/12 , G01N27/42
CPC分类号： C25D21/12 , C25D3/38 , G01N27/42
摘要： Suppressor and anti-suppressor additives in an acid copper sulfate plating bath are analyzed by the cyclic voltammetric stripping (CVS) method without cleaning or rinsing the cell between the two analyses. The suppressor analysis is performed first and the suppressor concentration in the resulting measurement solution is adjusted to a predetermined value corresponding to full suppression. This fully-suppressed solution is then used as the background electrolyte for the anti-suppressor analysis. This integrated analysis approach provides results comparable to those obtained with cell cleaning and rinsing between the analyses but significantly reduces the analysis time, consumption of expensive chemicals, and quantity of hazardous waste generated.
摘要翻译：酸性硫酸铜电镀浴中的抑制剂和抗抑制剂添加剂通过循环伏安法（CVS）方法进行分析，而不需要在两个分析之间进行清洁或冲洗。首先进行抑制分析，将所得测定溶液中的抑制浓度调整为对应于全抑制的规定值。然后将该完全抑制的溶液用作用于抗抑制剂分析的背景电解质。这种综合分析方法提供了与分析之间的细胞清洗和冲洗获得的结果相当的结果，但显着减少了分析时间，昂贵的化学品的消耗和产生的危险废物的数量。

2. 发明授权

US06890758B2 Measurement of complexing agent concentration in an electroless plating bath 有权
标题翻译：化学镀浴中络合剂浓度的测定
公开(公告)号：US06890758B2
公开(公告)日：2005-05-10
申请号：US10461652
申请日：2003-06-13
申请人： Eugene Shalyt , Michael Pavlov , Peter Bratin , Alex Kogan , Michael James Perpich
发明人： Eugene Shalyt , Michael Pavlov , Peter Bratin , Alex Kogan , Michael James Perpich
IPC分类号： G01N27/26 , G01N31/16
CPC分类号： G01N31/164 , Y10T436/116664 , Y10T436/173845 , Y10T436/174614 , Y10T436/19 , Y10T436/193333 , Y10T436/200833
摘要： The concentration of citrate complexing agent in an electroless cobalt or nickel plating bath is determined by titrating a sample of the electroless plating bath containing a small concentration of free fluoride ion with a standard lanthanum nitrate solution. During the titration, La3+ ion first reacts preferentially with the citrate complexing agent and then with fluoride ion, which reduces the free fluoride ion concentration. The endpoint for the titration is indicated by a substantial decrease in the free fluoride ion concentration, which is detected via a fluoride ion specific electrode (ISE). The method can be used for analysis of other complexing agents.
摘要翻译：通过用标准的硝酸镧溶液滴定含有少量游离氟离子的化学镀液的样品来确定无电镀钴或镍电镀浴中柠檬酸盐络合剂的浓度。在滴定过程中，La 3+离子首先优先与柠檬酸盐络合剂反应，然后与氟离子反应，这降低了游离氟离子浓度。通过氟离子特异性电极（ISE）检测到的游离氟离子浓度的显着降低来表示滴定的终点。该方法可用于其他络合剂的分析。

3. 发明授权

US06673226B1 Voltammetric measurement of halide ion concentration 失效
标题翻译：卤离子浓度的伏安测量
公开(公告)号：US06673226B1
公开(公告)日：2004-01-06
申请号：US10325334
申请日：2002-12-20
申请人： Alex Kogan , Eugene Shalyt , Peter Bratin , Michael Pavlov , Michael James Perpich
发明人： Alex Kogan , Eugene Shalyt , Peter Bratin , Michael Pavlov , Michael James Perpich
IPC分类号： G01N2726
CPC分类号： C25D21/12 , G01N27/42 , Y10T436/153333 , Y10T436/193333
摘要： The concentration of chloride ion in an acid copper electroplating bath is determined from the effect that chloride exerts on the copper electrodeposition rate in the presence of organic additives. A cyclic voltammetric stripping (CVS) rate parameter is measured, before and after standard addition of a plating bath sample, in an acid copper electrodeposition solution containing little or no chloride and at least one organic additive. Cross contamination and waste disposal issues associated with the reagents and reaction products involved in chloride titration analyses are avoided. The method may also be applied to analysis of other halides (bromide and iodide) and other solutions.
摘要翻译：酸性铜电镀浴中氯离子的浓度由氯化物在有机添加剂存在下对铜电沉积速率的影响决定。在电镀浴样品标准添加前后，在含有很少或不含氯化物和至少一种有机添加剂的酸性铜电沉积溶液中测量循环伏安法剥离（CVS）速率参数。避免与氯化物滴定分析中涉及的试剂和反应产物相关的交叉污染和废物处理问题。该方法也可以应用于其他卤化物（溴化物和碘化物）和其它溶液的分析。

4. 发明授权

US07186326B2 Efficient analysis of organic additives in an acid copper plating bath 失效
标题翻译：酸性镀铜浴中有机添加剂的有效分析
公开(公告)号：US07186326B2
公开(公告)日：2007-03-06
申请号：US10856619
申请日：2004-05-27
申请人： Eugene Shalyt , Michael Pavlov , Peter Bratin , Alex Kogan , Michael James Perpich
发明人： Eugene Shalyt , Michael Pavlov , Peter Bratin , Alex Kogan , Michael James Perpich
IPC分类号： C25D21/14 , G01N27/26
CPC分类号： C25D21/12 , C25D3/38 , G01N27/42
摘要： Suppressor and anti-suppressor additives in an acid copper sulfate plating bath are analyzed by the cyclic voltammetric stripping (CVS) method without cleaning or rinsing the cell between the two analyses. The suppressor analysis is performed first and the suppressor concentration in the resulting measurement solution is adjusted to a predetermined value corresponding to full suppression. This fully-suppressed solution is then used as the background electrolyte for the anti-suppressor analysis. This integrated analysis approach provides results comparable to those obtained with cell cleaning and rinsing between the analyses but significantly reduces the analysis time, consumption of expensive chemicals, and quantity of hazardous waste generated.
摘要翻译：酸性硫酸铜电镀浴中的抑制剂和抗抑制剂添加剂通过循环伏安法（CVS）方法进行分析，而不需要在两个分析之间进行清洁或冲洗。首先进行抑制分析，将所得测定溶液中的抑制浓度调整为对应于全抑制的规定值。然后将该完全抑制的溶液用作用于抗抑制剂分析的背景电解质。这种综合分析方法提供了与分析之间的细胞清洗和冲洗获得的结果相当的结果，但显着减少了分析时间，昂贵的化学品的消耗和产生的危险废物的数量。

5. 发明授权

US08118988B2 Analysis of copper ion and complexing agent in copper plating baths 有权
标题翻译：铜电镀液中铜离子和络合剂的分析
公开(公告)号：US08118988B2
公开(公告)日：2012-02-21
申请号：US12012197
申请日：2008-01-31
申请人： Eugene Shalyt , Victor Ososkov , Michael Pavlov , Peter Bratin
发明人： Eugene Shalyt , Victor Ososkov , Michael Pavlov , Peter Bratin
IPC分类号： G01N31/16 , C25D21/16
CPC分类号： G01N31/164
摘要： A simple titration method involving a single copper ion titrant detected by a copper ion specific electrode provides the concentrations of both copper ions and bath complexing agent (ethylene diamine, for example) in alkaline copper electroplating baths of the type used to deposit or thicken copper seed layers on silicon wafers. Standard addition of an excess of a strong complexing agent (EDTA, for example) and back-titration with the copper ion titrant yields the bath copper ion concentration, and continued titration to a second endpoint, preferably after addition of hydroxide to adjust the pH of the analysis solution, yields the total concentration of bath complexing agent. Based on these analyzes, the concentration of free bath complexing agent may be calculated. The method also provides direct determination of the free bath complexing agent concentration via standard addition of excess bath complexing agent to a sample of the plating bath and titration with the copper ion titrant.
摘要翻译：通过铜离子特定电极检测到的单一铜离子滴定剂的简单滴定法，可提供用于沉积或增厚铜种子的碱性铜电镀浴中铜离子和浴络合剂（例如乙二胺）的浓度硅晶片上的层。标准加入过量的强络合剂（例如EDTA）和用铜离子滴定剂的反滴定产生浴铜离子浓度，并持续滴定至第二终点，优选加入氢氧化物以调节pH 分析溶液，产生浴络合剂的总浓度。基于这些分析，可以计算游离浴络合剂的浓度。该方法还通过向镀液样品中标准加入过量浴络合剂并用铜离子滴定剂滴定来直接测定游离液络合剂浓度。

6. 发明授权

US08535504B2 Analysis of an auxiliary leveler additive in an acid copper plating bath 有权
标题翻译：在酸性镀铜浴中分析辅助矫平剂添加剂
公开(公告)号：US08535504B2
公开(公告)日：2013-09-17
申请号：US13065939
申请日：2011-04-02
申请人： Michael Pavlov , Eugene Shalyt , Peter Bratin , Isaak Tsimberg
发明人： Michael Pavlov , Eugene Shalyt , Peter Bratin , Isaak Tsimberg
IPC分类号： C25D21/14 , C05D5/00
CPC分类号： C25D21/12 , C25D5/04 , C25D17/10 , C25D17/12 , G01N27/48
摘要： An auxiliary leveler additive that cannot be analyzed by conventional CVS methods for acid copper plating baths is analyzed by cyclic voltammetry at a platinum rotating disk electrode from its effect on the anodic current at very positive potentials.
摘要翻译：通过常规CVS方法对酸性镀铜浴进行分析的辅助矫平剂添加剂，通过循环伏安法在铂旋转圆盘电极上的分析，从而对阳极电流产生非常正电位的影响。

7. 发明申请

US20090065362A1 Chloride analysis in acid copper plating baths 有权
标题翻译：酸性镀铜浴中的氯化物分析
公开(公告)号：US20090065362A1
公开(公告)日：2009-03-12
申请号：US11899787
申请日：2007-09-06
申请人： Michael Pavlov , Eugene Shalyt , Peter Bratin
发明人： Michael Pavlov , Eugene Shalyt , Peter Bratin
IPC分类号： C25D21/00 , C25D17/00 , G01N27/26
CPC分类号： G01N27/42 , C25D21/14
摘要： The chloride concentration in an acid copper plating bath is determined from the chloride oxidation current measured under controlled hydrodynamic conditions at a noble metal electrode using specific voltammetric parameters. The measurement is made directly on the undiluted plating bath so that the chloride measurement is fast and no waste stream is generated.
摘要翻译：酸性镀铜浴中的氯化物浓度由使用特定伏安参数在贵金属电极的控制流体动力学条件下测量的氯化物氧化电流确定。直接在未稀释的电镀槽上进行测量，以使氯化物测量速度快，不会产生废液流。

8. 发明申请

US20090057151A1 Detection of additive breakdown products in acid copper plating baths 有权
标题翻译：酸性镀铜浴中添加剂分解产物的检测
公开(公告)号：US20090057151A1
公开(公告)日：2009-03-05
申请号：US11895836
申请日：2007-08-27
申请人： Eugene Shalyt , Michael Pavlov , Peter Bratin
发明人： Eugene Shalyt , Michael Pavlov , Peter Bratin
IPC分类号： G01N27/26 , C25D21/00
CPC分类号： G01N27/42 , C25D3/38 , C25D21/12
摘要： An additive breakdown product in an acid copper plating bath sample is detected by performing a voltammetric analysis for the leveler additive in two measurement solutions comprising different volume fractions of the copper plating bath sample in a background electrolyte. When the plating bath sample contains a substantial concentration of the additive breakdown product, the analyses for the first and second measurement solutions indicate different concentrations for the leveler additive in the plating bath sample. A comparison of the leveler additive concentrations indicated by the two analyses provides a measure of the concentration of the additive breakdown product.
摘要翻译：在酸性镀铜浴样品中的添加剂分解产物通过对背景电解质中包含不同体积分数的镀铜浴样品的两种测量溶液中的矫味添加剂进行伏安分析来检测。当电镀浴样品含有相当浓度的添加剂分解产物时，第一和第二测量溶液的分析表明电镀浴样品中矫味剂添加剂的浓度不同。通过两个分析指示的平衡剂添加剂浓度的比较提供了添加剂分解产物的浓度的量度。

9. 发明申请

US20050247577A1 Detection of an unstable additive breakdown product in a plating bath 失效
标题翻译：检测电镀液中不稳定的添加剂分解产物
公开(公告)号：US20050247577A1
公开(公告)日：2005-11-10
申请号：US10838803
申请日：2004-05-04
申请人： Michael Pavlov , Eugene Shalyt , Peter Bratin
发明人： Michael Pavlov , Eugene Shalyt , Peter Bratin
IPC分类号： G01N27/26 , G01N27/42
CPC分类号： G01N27/42 , C25D3/38 , C25D21/12
摘要： The 3-mercaptopropylsulfonic acid (MPSA) breakdown product of the bis(sodiumsulfopropyl)disulfide (SPS) additive used in acid copper plating baths accelerates copper electrodeposition and can be detected by cyclic voltammetric stripping (CVS) analysis. In the presence of oxygen, MPSA decomposes rapidly in acid copper sulfate baths so that the CVS stripping peak area (Ar) decreases on successive cycles. The slope of a plot of Ar vs. CVS cycle number (or time) or logarithm of the CVS cycle number (or time) provides a measure of the initial MPSA concentration.
摘要翻译：在酸性电镀浴中使用的双（钠硫基丙基）二硫化物（SPS）添加剂的3-巯基丙磺酸（MPSA）分解产物加速了铜电沉积，并可以通过循环伏安剥离（CVS）分析来检测。在存在氧气的情况下，MPSA在酸性硫酸铜浴中快速分解，使得CVS剥离峰面积（连续循环）在连续循环中降低。 A 的曲线的斜率。 CVS循环数（或时间）的CVS循环数（或时间）或对数提供初始MPSA浓度的量度。

10. 发明申请

US20110266154A1 Analysis of an auxiliary leveler additive in an acid copper plating bath 有权
标题翻译：在酸性镀铜浴中分析辅助矫平剂添加剂
公开(公告)号：US20110266154A1
公开(公告)日：2011-11-03
申请号：US13065939
申请日：2011-04-02
申请人： Michael Pavlov , Eugene Shalyt , Peter Bratin , Isaak Tsimberg
发明人： Michael Pavlov , Eugene Shalyt , Peter Bratin , Isaak Tsimberg
IPC分类号： C25D21/12 , G01N27/416
CPC分类号： C25D21/12 , C25D5/04 , C25D17/10 , C25D17/12 , G01N27/48
摘要： An auxiliary leveler additive that cannot be analyzed by conventional CVS methods for acid copper plating baths is analyzed by cyclic voltammetry at a platinum rotating disk electrode from its effect on the anodic current at very positive potentials.
摘要翻译：通过常规CVS方法对酸性镀铜浴进行分析的辅助矫平剂添加剂，通过循环伏安法在铂旋转圆盘电极上的分析，从而对阳极电流产生非常正电位的影响。

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