公开(公告)号：US06733656B2

公开(公告)日：2004-05-11

申请号：US10115539

申请日：2002-04-03

申请人： Gene Chalyt ,  Peter Bratin ,  Michael Pavlov ,  Alex Kogan ,  Michael James Perpich

发明人： Gene Chalyt ,  Peter Bratin ,  Michael Pavlov ,  Alex Kogan ,  Michael James Perpich

IPC分类号： G01N2748

CPC分类号： C25D21/12 ,  G01N27/4163

摘要： In the present invention, the test reference electrode used for voltammetric analysis of a plating bath is calibrated relative to the zero-current point between metal plating and stripping at a rotating platinum disk electrode in the plating bath supporting electrolyte. This calibration is readily performed during the normal course of cyclic voltammetric stripping (CVS) or cyclic pulse voltammetric stripping (CPVS) plating bath analysis the need for additional instrumentation or removal of the test reference electrode from the analysis equipment. Automatic calibration of the reference electrode enabled by the present invention, saves labor, time and expense, and minimizes errors in the plating bath analysis.

摘要翻译： 在本发明中，用于电镀液伏安分析的试验参比电极相对于在电镀浴支持电解质中的旋转铂盘电极处的金属电镀和剥离之间的零电流点进行校准。 在循环伏安剥离（CVS）或循环脉冲伏安剥离（CPVS）电镀浴分析的正常过程中，这种校准很容易进行，需要额外的仪器仪表或从分析设备中去除测试参比电极。 通过本发明实现的参考电极的自动校准，节省人力，时间和成本，并最大限度地减少电镀浴分析中的误差。

公开(公告)号：US06749739B2

公开(公告)日：2004-06-15

申请号：US10266006

申请日：2002-10-07

申请人： Gene Chalyt ,  Peter Bratin ,  Michael Pavlov ,  Alex Kogan ,  Michael James Perpich

发明人： Gene Chalyt ,  Peter Bratin ,  Michael Pavlov ,  Alex Kogan ,  Michael James Perpich

IPC分类号： G01N2726

CPC分类号： G01N27/42 ,  C25D21/12

摘要： Relative concentrations of active suppressor additive species and suppressor breakdown contaminants in an acid copper electroplating bath are determined by cyclic voltammetric stripping (CVS) dilution titration analysis using two negative electrode potential limits. The analysis results for the more negative potential limit provide a measure of the suppressor additive concentration alone since the suppressor breakdowvn contaminants are not effective at suppressing the copper deposition rate at the more negative potentials. The analysis results for the less negative potential limit provide a measure of the combined concentrations of the suppressor additive and the suppressor breakdown contaminants. Comparison of the results for the two analyses yields a measure of the concentration of the suppressor breakdown contaminants relative to the suppressor additive concentration.

摘要翻译： 通过使用两个负极电位极限的循环伏安法汽提（CVS）稀释滴定法测定酸性铜电镀浴中的活性抑制剂添加物种类和抑制分解污染物的相对浓度。 由于抑制剂破坏污染物在抑制更多负电位下的铜沉积速率方面无效，所以对负电位极限的分析结果提供了单独的抑制添加剂浓度的量度。 阴极电位极限的分析结果提供了抑制剂添加剂和抑制分解污染物的组合浓度的量度。 两个分析结果的比较产生了抑制剂击穿污染物相对于抑制剂添加剂浓度的浓度的量度。

公开(公告)号：US06709561B1

公开(公告)日：2004-03-23

申请号：US10288989

申请日：2002-11-06

申请人： Michael Pavlov ,  Gene Chalyt ,  Peter Bratin ,  Alex Kogan ,  Michael James Perpich

发明人： Michael Pavlov ,  Gene Chalyt ,  Peter Bratin ,  Alex Kogan ,  Michael James Perpich

IPC分类号： C25D2112

CPC分类号： C23C18/1617 ,  G01N27/42

摘要： The concentration of a reducing agent in an electroless bath for plating a first metal is determined from the effect of the reducing agent on the electrodeposition rate of a second metal. For electroless cobalt and nickel baths, a sample of the electroless plating bath is added to an acid copper plating solution and the copper electrodeposition rate is measured by cyclic voltammetric stripping (CVS) analysis. Separate analyses for hypophosphite and dimethylamineborane in baths employing both reducing agents are attained via selective decomposition of the dimethylamineborane in acidic solution.

摘要翻译： 用于电镀第一金属的无电镀浴中的还原剂的浓度由还原剂对第二金属的电沉积速率的影响决定。 对于无电镀钴和镍浴，将化学镀浴的样品加入酸性镀铜溶液中，并通过循环伏安剥离（CVS）分析测量铜电沉积速率。 通过在酸性溶液中选择性分解二甲胺硼烷可以获得使用两种还原剂的浴中次亚磷酸盐和二甲胺硼烷的独立分析。

公开(公告)号：US06572753B2

公开(公告)日：2003-06-03

申请号：US09968202

申请日：2001-10-01

申请人： Gene Chalyt ,  Peter Bratin ,  Michael Pavlov ,  Alex Kogan ,  Michael James Perpich

发明人： Gene Chalyt ,  Peter Bratin ,  Michael Pavlov ,  Alex Kogan ,  Michael James Perpich

IPC分类号： G01N2726

CPC分类号： C25D21/12 ,  C25D3/38

摘要： Acid copper electroplating baths used to form ultra-fine circuitry features on semiconductor chips contain suppressor, anti-suppressor and leveler additives that must be closely controlled in order to obtain acceptable copper deposits. Cyclic voltammetric stripping (CVS) methods are available to measure the concentrations of the suppressor and anti-suppressor based on the effects of these additives on the copper electrodeposition rate. The present invention is a method that also uses measurements of the copper electrodeposition rate to determine the concentration of the leveler additive. The other two additives are included in the measurement solution at concentrations determined to provide the optimum compromise between minimal interference, high sensitivity and good reproducibility for the leveler analysis. In this case, measurement precision is greatly improved compared to that provided by inclusion of the interfering additives in the measurement solution at their concentrations in the bath sample at the time of the analysis, which would be the standard analytical procedure.

摘要翻译： 用于在半导体芯片上形成超细电路特征的酸性铜电镀浴包含必须严密控制的抑制剂，抗抑制剂和矫味剂添加剂，以获得可接受的铜沉积物。 基于这些添加剂对铜电沉积速率的影响，循环伏安法（CVS）方法可用于测量抑制剂和抗抑制剂的浓度。 本发明是还使用铜电沉积速率的测量来确定矫光添加剂的浓度的方法。 其他两种添加剂被包括在测量溶液中，其浓度被确定为在矫正剂分析的最小干扰，高灵敏度和良好的再现性之间提供最佳折中。 在这种情况下，与在分析时在浴样品中浓度测定溶液中包含干扰添加剂所提供的测量精度相比，测量精度大大提高，这将是标准分析程序。